M.E.TEK revised w/pics

Discussion in 'Cacti Delecti' started by ancient powers, Apr 9, 2008.

  1. ancient powers

    ancient powers Member

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    Let us first begin by identifying the varieties (var) that we are going to be discussing. There are 3 var in particular of the San Pedro Cactus that we will be discussing. Trichocereus Pacahanoi, Peruvian, Bridgesii. So far these are the ones reported to have entheogenic psychoactivity and the ones in which we will be discussing. The techniques described apply to all 3 var. T. Macrogronus has yet to become a common ally among the 3 var. as of now. Further reseach, study, cultivation and extraction will yield the needed data for the future. San Pedro is interpreted into St. Peter who is keeper of the gates of heaven. So the cacti is the key to enter into through the gates or veil to the eternal awareness of the never ending moment.

    Step 1. Growing a Cutting.

    This is by far the easiest step. The thing about the cutting is that it can remain alive for a long time as a cutting out of soil. I have not tested a cutting to suffer a long death for the data, but I do know it will start growing pups even out of soil.

    The best place to start is an online vendor otherwise you will have to harvest a cutting from a neighboring yard. The average price for a cutting is about $25 per foot. I know the pachanoi var grows in many neighborhoods of the southern california region. I seldomnly come across pervian or bridgesii, but I have. And when the day comes that I can grow the sacred cacti in my own yard I will. For now I wait and allow them to grow free. On a journey through phoenix Az. I did happen to spot more peruvian var then the other two.

    A 1ft cutting is standard to start growing and using sacred cacti. Simply plant the cutting directly into common potting soil or cactus potting soil and start watering. You should start with a 3-5g plastic pot. Plastic pots work the best due to the fact that they retain moisture longer then clay. I've noticed that the San Pedro var. cacti grow best in indirect sun with plenty of watering, but they can handle full sun as long as they get plenty of water. Lack of water seems to make them prune up and in full sun they become yellow. The most potent samples you are going to want to use for brewing/extracting are going to be the darkest green and very juicy.

    Every cutting that was less then a foot that I had planted always grew pups on the top and the cutting only remained a base. Once any cutting has established roots it will begin to grow pups out the base. For cuttings that are not tops there is a way of cloning from these that I have observed. What you want to do is cut the cutting into 2-3in long chunks and plant them half deep on their sides in 1g plastic pots. The pups always grow out the side that would have been the top end of the cutting. For example if you layed a 5ft cutting on the ground and let it sprout a pup. It would grow out the part of the cutting that was its most top part and the remaining 5ft of cacti will not sprout any pups. Whereas if you cut 5ft into 30x2in chunks you could sprout 30 pups. The rule is confirmed that the cacti grow about 1ft+ a year once the roots are established and have plenty of room and watering.
     
  2. ancient powers

    ancient powers Member

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    To grow from seeds you are going to need to practice patience. If you want to breed the cacti to produce viable seeds you are going to need to grow cacti from seed and grow them only to produce seeds. For single seed growth I recommend those cactus growing kits from your local home improvement center. If you want to grow alot at once take a 1ftx1ft garden flat fill it with cactus soil mix or potting soil, pre water, sprinkle your seeds throughout and keep in a warm and well lit space out of direct sunlight.. Make sure they get a good dose of partial sun. Full sun will be way to intense. I would also wait till spring before planting so there is no chance of cold killing em off during the sprouting cycle.

    Allow the cacti to grow to a decent size before transplanting them to larger pots. If you are growing to produce seed stock for the future you are going to want to use organic gardening techniques to optimize growth to produce healthy, potent viable seeds. Once your seed sprout cacti transplants have grown to 3in-6in, Its time to plant them into mother earth. Your are going to want to dig a 4ft-5ftx4ft-5ft hole in the ground and fill the hole with your soil mixture. 1part manure/compost 1part soil of the earth which you removed from the hole. This ensures that the roots will have plenty of room to grow without any fighting to establish. And the soil will be sure to have plenty of nutrients and nitrogen to produce very dark green, healthy stocks. Use a drip system to water them every evening and a little each morning. Make sure they don't get too much water and not enough of it. You need to find a perfect balance.

    Make a cover with screening used to reduce UV to provide optimum partial shade in full sun. They way alot of nurseries do it. Once the cacti reach 3ft-4ft they will begin to flower. The flower begins as a grey fuzzy pod. As long as the cacti recieve ample amount of H2o, the cacti will flower. If you are farming anything for seeds you will need to do some research into raising your own bees in a designated spot near your farm. As long as there are plenty of bees to pollinate you will produce seeds. You can do it by hand with a q-tip but that is for small amounts of flowering cacti and no ample bee supply.

    The flowers only last 3 days. If they do not get pollinated the whole flower will fall off. If there was pollination then the flower will fall leaving a seed pod to be left on the cacti until the pod begins to break open. At this point remove the pod and open it to remove the seeds. The seeds are very small and black similar to poppy seeds and they are kept in a white slimy bed within the pod. Just use the tip of a knife to remove them from the bed.
     
  3. ancient powers

    ancient powers Member

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    When harvesting your cacti you will always want to cut as close to the base as possible to ensure strong new growth from the roots. The top 1ft of the harvested column should always be planted out of respect for the cacti to ensure its survival and to sow for a future harvest. But do what thou wilt.

    The nest step is to despine the harvested cactus. This is done by cutting two tiny 45 degree cuts on underneath the spine so that the cuts meet underneath the spine to remove it. The harvested and despined columns are then washed in cold water.

    When using pachanoi var. there is no need to bother removing the spines since they are relatively so small. Also tin snips or sharp shears should be able to cut the larger spines on peruvian/bridgesii var. If the dried skins are used for extraction purposes having spines with the skins is fine except that it may throw off the weight of valuable product by a minute fraction and the pricks can hurt.

    What you are going to need to do is cut off all the spines first. Wash the cactus and begin to cut up the cactus into 3in sections. Then begin to cut off the outer dark green layers of the sections.

    Lay out a large cardboard or plywood and place all the skins skin side down with the dark green flesh up in full sun for 5-7days. You can use a conventional oven on the lowest setting using baking sheets skinside down. This takes a long while and makes your place reek of cacti!

    Shred the dried skins in a blender, then powder them in a coffee grinder. You get like 50g powder to the 1foot of SP var. so 40ftx50gs = 2000g or 4.5lbs. Thats about 20g-40gs alkaloids. pachanoi-peruvian/bridgesii.
     
  4. ancient powers

    ancient powers Member

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    For a large cook I would advise cooking out the alkaloids using 1tbsp vitamin c powder or citric acid per 1liter of water. Use the blender shredded skins for this cook. It is alot easier to strain out the pulp in the shredded form. In a large stainless steel cooking pot add your SP powder and vitamin c water until it becomes very soupy.

    Simmer the soupy mixture for 20min with frequent stirring. Use the lid to help pour off the cooked water without getting any cactus matter into the solution. Pour into a seperate container and refresh the pot with fresh vitamin c water. Cook powder 3x to extract all water soluble alkaloids.

    Filter extract solution and use 1 gallon ziplock baggies to seperate sediment out of solution. Hang baggie up by one corner and allow sediment to sttle overnite. Next day snip a small hole in the bottom corner and gently massage sediment through the hole with your fingers.

    Reduce your solution on a low simmer then evaporate the reduced solution on a large glass baking dish in oven at lowest setting to a wet solid. Allow wet solid to dry at room temp. Scrape and consume as is or make into a purified salt form using the a/b tek below.

    1/2lb (224gs) of San Pedro var. Cactus powder is added to a clean 2 quart plastic HDPE2 ammonia bottle.

    1500ml of tap water is added to the bottle and shaken.

    6tbsps of NaOH(lye) is added using a funnel 1tbsp at a time. Cap and shake bottle after each tbsp to distribute NaOH(lye) evenly and to avoid melting the bottle.

    500ml d-limonene or xylene solvant is added to bottle using a funnel which will fill the bottle to maximum capacity. Make sure to leave a little air bubble at the top to help with the mixing process. Cap and shake bottle as much as you can the first day and let sit over night.

    The strong alkaline cactus solution will shrink a bit over night so you will need to add a little more solvant the next day, shake again and let seperate.

    Drill a hole in a spare cap and feed a 3ft long piece of 3/8in clear vinyl tubbing at 8 and 1/4cm long from the bottom of the cap to siphon off the solvant.

    Cap and siphon solvant into a pint glass Ball mason jar. Make sure to only get solvant and no cacti solution. Some solvant will be left behind in the solution bottle. 300ml to 400ml of solvant is perfect for salting.

    Add 1tbsp NaOH(lye) to the cactus solution using a funnel, cap and shake.

    Add 2oz of distilled water to the jar of siphoned solvant and 2 drops of hardware store brand 31.45% muratic acid(HCl) using a tincture dropper and shake for 5min. Seperate layers in a quart ziplock freezer baggie or freeze hcl extract layer solid by putting jar in the freezer.

    Hang baggie up by one corner and carefully snip a small hole in the bottom corner to slowly drain the bottom clear to foamy layer into a clean ball mason jar.

    Drain the solvant layer back into the solution bottle, cap and shake for 5min then let seperate. At this point the solution will seperate in a few minutes.

    Shake and let seperate a few times to maximize extraction yields.

    Extract the cactus solution 4x. One right after the other. Do not wait another day. All extractions after the first day of seperation need to be perfomed back to back to ensure the highest purity from cactus fats and oils. After a few days of sitting and seperating, the solvant layer absorbs fatty oils that make the 2oz hcl water layers foamy instead of clear.

    All 4 hcl water extraction layers are collected together in a jar of 200ml fresh solvant and shaken repeatedly to wash the hcl extract solution. This will help remove any solvant soluble materials that may have polluted the hcl extract solution layer. The mixture is seperated with freezing.

    Make sure to remove the frozen hcl layer to evaporation(evap) dish before it melts or you will be scraping excess crystals off the inner jar.

    The hcl extract solution is evaporated on a large glass baking dish, using a fan or 150F oven. Fan evaporation will ensure that you do not damage the product. The oven is great for testing to see if alkaloids will crystal from the material being used or if the extractors are in a hurry.

    Pack into '0' gelatin capsules.

    Refer to ekstanza's tek for more regarding this method.
     
  5. ancient powers

    ancient powers Member

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    https://www.youtube.com/watch?v=3lnJ0uvbSK8"]https://www.youtube.com/watch?v=3lnJ0uvbSK8
     
  6. ancient powers

    ancient powers Member

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    Gather a handful of MGS which is about 24gs, 600 seeds, or 6mg alkaloids. This is enough for a full spectrum dose. Grind seeds into a powder with a coffee grinder. Add a double volume of distilled water to the volume of seeds, shake and let sit in the fridge for 1hr with shaking every 15min. Strain carefully through fine mesh and toss the seed pulp. Clean the fine mesh and restrain the solution until no sediment remains. Consume Holy Water on an empty stomach eating oranges to neutralize the taste of the potion.
     
  7. ancient powers

    ancient powers Member

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    Clean 100HBWRS using your fingernails to remove the fuzzy coating. Grind the cleaned seeds in a coffee grinder and soak powder in double the volume of powder with vodka. Soak in the freezer for 30min with shaking after 15min. Carefully pour off vodka solution through fine mesh leaving the sediments. Refill with double the volume and repeat with freezing for 30min, shaking after 15min and carefully pour off solution through fine mesh leaving the sediment settled in the bottom of the jar.

    Filter the 2 solutions together though fine mesh until no sediment remains. Put solution in a ziplock baggie and hang. Allow the sediment to settle and seperate them out by cutting a small hole in the bottom corner. Collect the solution layer only. Evaporate the solution with fan on a large glass baking dish in a cool dark place.

    Simply scrape dried residue and reconstitute in 25ml fresh vodka for a 1oz tincture of 1ml per 1mg alkaloids. That is 25 doses. Use 3-6ml droppers for full effects.
     
  8. ancient powers

    ancient powers Member

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  9. ancient powers

    ancient powers Member

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    Acid-Base Extraction of Mescaline from San Pedro

    by Prdy2GO and starlight, HTML by metanoid [ Back to the Chemistry Archive ]

    Prdy2GO:

    Step 1: Aqueous Extraction

    First, you need to prepare a "tea" from your cacti. If using dried cactus, powder it. If using fresh cactus, chop it to small pieces and then puree it in a blender. At this point, it is a good idea to weigh your cactus and record the weight. This will be helpful further on in the process. Put the cactus in your stainless steel pot and cover with just enough water to make a soup. Add some acid to make the pH of the soup fairly acidic. If using citric acid, you want to add about 3 grams per liter of water. Boil the cactus about 20 minutes. If you use sufficiently acidic water, there is no need to boil longer than this. After boiling, strain out the cactus chunks (the marc) and save the liquid. You want to do three acidic water extractions on the cactus. Combine the 3 liquids and toss the marc on your compost pile or dispose of it in some other non-wasteful manner. If the volume of liquid you have is large, you may want to boil it down to a more managable quantity.

    Step 2: De-Fatting

    Once cooled, the next step is to de-fat the solution. This step will remove the fats and many other non-alkaloidal plant matter. Make sure the solution is acidic (pH 4 is good) before doing this. If the solution is acidic, the alkaloids will be in a salt form which is soluble in water but not in xylene. Pour the solution into a glass jar (or separatory funnel, if available). Add 25-50% of the solution volume in xylene. For example, if you have 200ml of solution, add 50-100ml of xylene. Put the lid on the jar and gently turn the jar over 50 to 100 times. Do not shake the mixture vigorously as this could result in emulsions that will be difficult to separate. (If you do end up with an emulsion layer, which looks like a thin layer of poorly separated bubbles, bathing the jar in hot water can help separate the emulsion. If the emulsion layer is thin enough, you may wish to just discard it rather than taking the time to let it separate.) Once mixed, let the jar sit and separate out into the different layers. When this is done, you will have a top layer of solvent, a middle fatty layer, and a bottom layer containing the acidic aqueous solution (and the alkaloids).

    If you are using a separatory funnel, drain out the bottom aqueous layer and throw away the top two layers. Alternatively, use a turkey baster to siphon off the top two layers and discard them. (Make sure you dispose of all solvents safely! Do not flush it down the toilet if you have a septic tank. If pouring it down a sewer-connecting drain, make sure to wash it down with large amounts of water.) You will likely find that the turkey baster only gets off most of the solvent and fat layers. To get the thin layer that the turkey baster can't get, try this trick. Siphon off all of the remaining solvent and fat layers, as well as some of the top of the aqueous layer. Put this liquid into a tall thin glass container (a graduated cylinder or test tube, for example), and let it separate back into layers. Then, use an eye dropper to get off the solvent and fat layers, then add the remaining aqueous solution back to the main jar.

    There is one other possibile approach to separating the layers. Because xylene freezes at -47.7 degrees Celsius, a separation can be done in the freezer. Put the container in the freezer and let it sit for a few hours until the water has frozen solid. The xylene can then be poured off and discarded. I do not know if this will work for defatting, as I do not know the freezing point of cactus fats. If the fats freeze at freezer temperatures, it may not be possible to pour them off with the xylene. This freezing technique can certainly be used later on in steps 4 and 5 to separate the xylene and water layers, however.

    Repeat the de-fatting process two more times, or until you no longer get a fatty layer after separation. Make sure that you have good ventilation through the whole de-fatting process (or any time you are working with xylene). If you begin to feel light-headed or nauseous, or get a headache, go outside immediately and breathe fresh air until you feel better. Also, make sure there are no open flames or sparks as xylene is quite flammable.

    Step 3: Basification

    After de-fatting, slowly add sodium hydroxide to the aqueous solution until the pH is up around 10. Rather than adding dry sodium hydroxide, it may be wise to prepare a solution of sodium hydroxide in water, and add this. Be careful when mixing the sodium hydroxide and water, as the mixture will cause an exothermic (heat producing) reaction. Do not prepare the mixture in heat-sensitive containers. When working with sodium hydroxide, remember that it is a highly caustic material and can burn you badly. Avoid contact, especially with the yes, and if any gets on you wash the spot immediately with plenty of water. It is highly recommended that you wear protective gloves and goggles when working with sodium hydroxide or other hazardous chemicals.

    Be aware that once you do this step, you need to continue the extraction at least up through the xylene extraction because leaving the alkaloids in a strongly basic solution will cause them to start breaking down after several hours. Making the solution basic turns the alkaloids into their free base forms, which are soluble in xylene.

    Step 4: Extraction of Free Bases

    Once the solution is basic, xylene using the same ratio as used during the de-fatting process. Again, mix the solution thoroughly but gently to avoid emulsions. Let the solution sit, and it will separate out into two layers. On the bottom will be a basic aqueous solution, and on the top will be a xylene layer which now contains the alkaloids. Using either a separatory funnel or a siphoning process, collect the xylene layer and set it aside. Since there will still be significant alkaloids in the aqueous layer, repeat this process two more times. Combine all the xylene and discard the remaining aqueous solution.

    If you are using a separatory funnel, gas may be formed when adding xylene to the basic solution. To prevent pressure from building up and potentially leading to an explosion, vent the separatory funnel occasionally. If you are using a jar, you should remove the lid.

    Step 5: Salt Formation and Extraction

    The next step is to add acidic water to the xylene. This will cause the alkaloids to convert to their salt forms, which are soluble in water but not xylene. If using hydrochloric acid from the hardware store, it will already be diluted and may be usable as is. Read the label to find the concentration. One source says, "HCl from the hardware store is generally between 24%-36% HCl. This is far from dilute. Indeed, upon opening the container, a visible plume of white vapor can be seen creeping out of the bottle. First the lungs start to burn, then any skin which is exposed to the air starts to sting... This should be diluted, especially if it is going to be worked with without a fume hood. 20 drops acid per 500ml of water may even be sufficient."

    If using vinegar (acetic acid), it comes quite diluted (around 5%) and should be used as is. It would probably be best to use plain white vinegar. I do not know what else is in vinegar other than water and acetic acid, but it is likely other chemicals remain from the original wine, and this may affect your final product. There should not be any harmful products from using vinegar, since it is a food-safe product, but you may not get nice crystals after evaporation.

    If using citric acid (which is the recommended choice), prepare a solution of citric acid powder with a small amount of water. I recommend using citric acid because unlike hydrochloric acid, it is food-safe and safe to handle, and unlike either hydrochloric acid or vinegar, it is available in pure form. I have been told that using hydrochloric or acetic acid has the advantage that both are volatile and that excess will evaporate off, unlike citric acid. However, since neither are easily available in pure form, it is still probably better to use citric acid. Beware that if you do use hydrochloric acid and let it evaporate, the fumes can be hazardous and the evaporation should not be done where you might breathe in the vapors.

    For this step, it is useful to have some idea how much alkaloid should be in your cactus extract. If you weighed your cactus before extraction.

    Trichocereus pachanoi has been analyzed with mescaline contents of 0.025-0.12% fresh weight (0.331-2.0% dry weight). Mescaline is usually around 50% or more of total alkaloid content. You will want to add an equimolar quantity of acid to the solution.

    If you can't or don't want to estimate the alkaloid content, Trout gives the following work-around: add very small quantities of acidic water to the xylene, let separate, and then collect the water layer. Check the pH of the water, and it should be neutral. Repeat this with small batches of acidic solution until the water layers come out acidic. Trout points out that "Something to keep in mind is that neutralization won't always be immediate. pH should be checked after a few minutes to see how it is, adjusted if needed and rechecked a few minutes later."

    If you are using citric acid and you are not worried about having citric acid powder in the final product, you can just add enough acidic water to make the solution slightly acidic, and repeat this once or twice, then combine the extracted water layers. As citric acid is both food-safe and a solid powder, this is a sloppy but safe approach. Shulgin suggests that this may be a better approach than stopping when the water layers stop coming out neutral: "My gut feeling is that there may be quite a bit of alkaloid still in the xylene, and maybe a couple of extracts with more aqueous acid would be useful. True, it may load the product down with excess citric acid, but the increased yield might be worth it."

    However you approach it, after the acidification and water extraction step, discard the xylene. Again, make sure to dispose of it in a safe manner.

    Theoretically, this step could be skipped entirely, and you could just let the xylene evaporate. This would leave behind mescaline (and the other alkaloids) in free bas form, which is an oil. This is not recommended however, as mescaline oil is highly caustic and it would burn your skin to touch it. Since its an oil, it would also not be possible to put into capsules. Perhaps you could put the oil into some acidic fruit juice and safely drink it, but it is still preferable to go through this step to produce a salt form. Perhaps it may even be smokable, though I know of no reports of anyone trying to smoke (or vaporize, rather) free base cactus alkaloids. The boiling point for mescaline free base is around 180 degrees Celsius. One final concern is that free base mescaline oil may not have the shelf life of a salt.

    Step 6: Evaporation

    Finally, pour the water into a large pyrex baking pan. Set it in a protected location to evaporate. Let it evaporate slowly at room temperature rather than using heat, as this will give you a better chance of producing nice crystals. After the water has fully evaporated, scrape up the crystals (or whatever solid mass you end up with) and put them in capsules or a vial for storage.

    Keep in mind that when measuring doses, there are a few things to consider. First, your extract will contain all the alkaloids from the cactus, not just the mescaline. Second, depending on what acid you used in step 5, you will have different salts of the alkaloids. For example, if you used citric acid, you will have mescaline citrate (as well as citrate salts of the other alkaloids). If you used vinegar, you will have mescaline acetate. If you used muriatic acid you will have mescaline hydrochloride. The doses of each will be slightly different, due to the different molecular weights of the different acids. Because of these factors, you will need to figure out the potency of your material before you can weigh doses accurately.

    Conclusion

    Do make sure that you follow all safety instructions religiously. Failure to excersize caution can easily lead to harm and even death. To stress this point even further, I will close with some comments from Trout:

    "It seems like it does not matter how many times you tell some people things, lots of them decide what THEY think is really important and items like solvent exposure and not using plastics or solvents stored in plastics (or even the use of slow and careful heating) get forgotten whenever it is not convenient to follow the instructions.

    Its very distressing how careless some people are. Worse, people like this often expose not just themselves but family, children and pets with no thought or concern.

    You would not believe some of the letters I have gotten. Some of them I almost can't shred fast enough.

    I'm sadly coming to believe that a simple citrate tea (lime not lemon) or else dried outer flesh consumed as powder are the only safe approaches the general public is capable of handling responsibly."

    References


    [1]Fletch. Private e-mail. December 7, 2001.
    [2]Shulgin, Alexander. Private e-mail. November 24, 2001.
    [3]Trout, K. "Sacred Cacti." Second edition, 1999: Chapters 4, 6 and 10.
    [4]Trout, K. Private e-mail. December 1, 2001.

    Starlight:

    crystallization using sulfuric acid

    Just replace steps 5 and 6 above with the step below:
    This method relies on the low solubility of mescaline sulfate in very cold water.

    (this is not tested from personal experience, but sourced from Trout: Sacred Cacti and Selected Succulents, 1997)

    Step 5: Salt Formation and Crystallization

    Once you have separated the organic solvent, dark (or in the case of recrystallization at least yellow) with alkaloid and impurities from the basic solution, extract it with dilute sulfuric acid. Use only as much as is required to neutralize the alkaloid bases. A little excess at this point is not desirable, but not of concern. Separate the small volume of aqueous solution now containing the mescaline sulfate and other alkaloid sulfates.

    It will need gentle heat to reduce it somewhat, but do not let it become thick, or overheat. Take this solution while warm and insulate it well (a small styrofoam shipping box will work as will being carefully wrapped in towels). Stick the whole thing in your refrigerator until quite cold (near 0C) but do not freeze.

    The object is to retard the rate of cooling to as slow as possible. This will cause the formation of large, beautiful crystals. If you chill rapidly a crystalline mush of many tiny crystals will form, trapping impurities.

    Take the mother liquor containing the crystals and pour through a buchner funnel. Allow the air to keep sucking through the crystals. Briefly squirt a bit of ice cold water through the crystals to rinse them of any remaining solution. Turn off the air flow briefly and immediately dump out the mother liquor and ice water rinsing and save.

    Rapidly resume air flowing through the Buchner. Then quickly rinse the crystals with a little acetone to remove the remaining water. Let the air keep flowing to pull off as much liquid as possible. (If one has access to a cold room all of this will be more efficient).

    Take the filter and immediately dry in a warm oven (120-120F) with the door open. Package as soon as dry and keep away from light, heat, moisture, air.
    Second and third crops of crystals may be obtained by reducing the mother liquor further (do not allow to become thick) and again chilled. By the third or fourth time other alkaloids will begin to crystallize. These may be grey in colour and have a plate-like structure. They should be easily distinguishable from the beautiful yellow or white needles and prisms of mescaline sulfate.

    The sulfate salt can be converted to the hydrochloride salt by acid base and evaporation if so required.
     
  10. ancient powers

    ancient powers Member

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    Extracting Pure Mescaline From Peyote or San Pedro Cactus From the Book: PEYOTE & Other Psychoactive Cacti by Adam Gottlieb 1977 Kistone Press Typed and Uploaded by Elric of Imrryr For more interesting and educational files call: Lunatic Labs UnLimited BBS 213-655-0691 1200/2400 ----------------------------------------------------------------

    The isolation of mescaline from cacti containing this alkaloid is not difficult to perform and is perhaps one of the most rewarding alchemical processes that one can attempt. The chemicals required for this process are readily avilable and their purchase arouses no suspicion or interest on the part of government agencies [This may no longer be true, use reasonable caution when purcahsing any chemicals - EoI]. The equipment employed is not expensive or particularly complicated or can be constructed very easily from ordinary household items. The entire process can be carried out in any kitchen in a matter of hours by following the instruction below and in the final stages one can verify the success of the procedure by actually watching the crystals of mescaline precipitate in the solution.
    One kilo (2.2 lbs.) of dried peyote buttons may yield between 10 and 60 grams of pure white needle crystals of mescaline depending upon the potency of the plants used. On the average the yield is about 20 grams. The usual underground price for a kilo of dried peyote ranges between $125 and $250 (25› to 50› per button). From Indians in the southwestern USA the price is closer to $50 (10› per button). The street price for a gram of pure mescaline is $20 to $30 - if one is lucky enought to find it. One can obtain from a kilo of peyote $200 to $1200 worth of mescaline. If San Pedro is employed one may anticipate a yield of 3 to 12 grams of mescaline per kilo of dried cactus. One can legally purchase a kilo of dried San Pedro for $5 to $10 and from it extract $60 to $250 worth of mescaline. [Note from Elric: The above prices are in 1977 dollars. Neither peyote or mescaline are commonly available these days, but San Pedro cactus is still legally avialble in most cactus stores.]

    PROCESS [NOTE!! In NO CASE should any aluminium cookware, containers, or utensiles be used at any point in the process. Stainless Steel is the best bet.] Grind a kilo of the cactus, place this in a large pressure cooker, cover with distilled water and boil for 30 minutes. Strain the liquids and save them. Return the pulp to the pot add more water and boil again for 30 minutes. Strain the liquids and combine with the first strainings. Repeat this process about five times or until the pulp no longer has a bitter taste. Discard the pulp and reduce the volume of the combined strainings by boiling in an open pot. Do not use aluminum ware.
    When the liquids have been concentrated to the thickness of cream (about 1 quart) stop the boiling and stir in 400 g of sodium hydroxide [Carefully and slowly, it will react with the liquid]. This makes the mescaline more soluble in benezene and less soluble in water. If a large separatory funnel is avilable pour the liquids into it and add to this 1600 ml of benezene [Carefully again]. Shake the funnel well for 5 minutes and let stand for 2 hours. If a separatory funnel is not available the process can be carried out in a one gallon jug with a siphon attached. After standing for 2 hours the water layer will settle to the bottom and the benzene layer will float to the top. Between the two layers will be a thin emulsion layer of mixed water and benzene. Drain off the water and emulsion layers if you are using a separatory funnel or siphon off the benzene layer if you are using the makeshift jug-siphon aooaratus. Be certain that neither the water or emulsion layers get into the benezene layer when separating. If any of these layers do get into the benzene during the separation, pour everything back into the separator, let stand and repeat the separation more carefully. It is better to leave some benzene layer in the water and emulsion than to get the water or emulsion in the benzene. Nothing will be wasted. All of the benzene which contains the mescaline will eventually be salavaged.
    Sometimes the layers will fail to separate properly. If this is the case immerse the funnel or jug in a deep pot of hot water for two hours. This will break up the emulsion and bring about the separation. Prepare a solution of 2 parts sulfuric acid and 1 part water. (Never add water to the acid or it will splatter; add the acid a little at a time to the water by pouring it down the inside of the graduate or measuring cup containing the water.) Add 25 drops of the acid solution one drop at a time to the benzene extracts. Stopper the jug and shake well for 1 minute. Thenlet it stand for 5minutes. White streaks of mescaline sulfates should begin to appear in the benzene. If these do not appear, shake the jug more vigorously for two or three minutes and let it settle for another 5 minutes. I have found that when extracting mescaline from San Pedro it is sometimes necessary to shake the mixture more thoroughly and for a longer time to get the mescaline streaks to form. This is probably because of the lower mescaline content in the plant. This would also apply to any peyote that does not have a high mescaline content. After the streaks appear add 25 more drops of the acid solution in the same manner, shake as before and let settle for 10 minutes. More streaks will appear. Add 15 drops of acid, shake and wait about 15 minutes for more streaks to form. Add 10 drops, shake and wait about 30 minutes. Test the solution with wide range pH paper. It should show that the solution is between pH 7.5 and 8. Allow the mescaline sulfate crystals to completely precipitate.
    Siphon off as much of the benzene as possible without disturbing the crystals on the bottom of the jug. The next steps are to salvage any mescaline still in the water and emulsion layer. Combine the benxene siphonings with the water/emulsion layer, shake these well together for 5 minutes and let settle for 2 hours as before. Carefully remove the benzene layer, treat it again with acid, precipitate the crystals and siphoned benzene with the watery layer and repeat this again and again until no more crystals precipitate. Siphon off as much benzene as possible without drawing crystals through the siphon.
    The next step involves removing the remaining benzene from the crystals. There are two methods to choose from. The first is the quickest, but requires ether, which is dangerious and often difficult to procure. Shake up the crystals with the remianing benzene and pour it into a funnel with filter paper. After the benzene has passed through the filter rinse the jug with 100 ml of ether to salvage any crystals in the jug and pour the ether over the crystals in the fitler. After the ether has passed through the filter repeat the rinsing with another 100 ml ether. Then let the crystals dry. If ether is not available or if you do not wish to use such a highly combustible substance, the precipate and residual benzene can be poured into a beaker. The jug should be rinsed several times with a little benzene and added to the beaker so that no crystals are left behind. The beaker is then placed in a heat bath until all of the benzene has been evaporated.
    The next step is to purify the mescaline sulfate crystals. After either of these methods has been carried out dissolve the dry crystals in 200 ml of near-boiling distilled water. Add a pinch of activated charcoal (Norite) and filter while still hot through #2 filter paper. The hot water which contains the mescaline will pass through the filter. The Norite absorbs impurities from the mescaline. After the liquids have passed through the filter pour a little more hot water over the filter to rinse through any remaining mescaline which may have impregnated the filter paper.
    Add 10% ammonia solution a few drops at a time to the hot filtrates until the solution registers between pH 6.5 and 7. Place a boiling stone in the solution and reduce its volume to 75 ml by boiling. Remove the boiling stone and allow the solution to cool to room temperature. Place the solution in a freezer or in a refrigerator turned up to the coldest possible temperature and the solution to cool almost to freezing. Tiny white needle like crystals will form around the bottom and sides of the beaker. Break up the crystals with a glass stiring rod while the solution is still ice cold and pour through a filter. Mescaline sulfate is insoluble in near freezing water and will not pass through the filter. Rinse the beaker with fresh ice water and pour this over the filter. The crystals will now be pure white and can be dried under a heat lamp or in an oven at 250� F. More mescaline can be salvaged from the water that has passed through the filter by boiling these liquids down to about 20 ml. adding Norite while hot, filtering through #2 paper as before, chilling the filtrate to near freezing once more, filtering while cold, rinsing with ice water and drying the crystals. This repetition should obtain at leat 2 more grams of mescaline sulfate. If large volume mescaline extraction is being conducted it would be worthwhile to repeat this salvaging procedure several more times.
     
  11. ancient powers

    ancient powers Member

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    Mescaline Extraction Tek
    --------------------------------------------------------------------------------
    This is an excellent extraction tek. All credit goes to Ekstaza for the pictures and text. This is the simplest full extraction that I've found. It doesn't require a seperatory funnel and it's written in simple step-by-step recipe style wording. This was written to accommodate people who don't understand the chemistry completely. All of the steps are for the sole purpose of extracting mescaline and turning it into mescaline hcl.

    Items you'll need

    1. At least 2 glass or HDPE(should show a triangular recycle symbol with a 2 inside of it somewhere on the bottom) plastic jugs or jars. HDPE is preferred because strong lye solutions will etch glass and cause it to break eventually. I know first hand.
    2. RedDevil brand lye
    3. Muriatic acid (HCL or hydrochloric acid)
    4. Acetone
    5. Xylene
    6. turkey baster
    7. a glass or stainless steel funnel
    8. cotton balls
    all easy to get items (use NO aluminum)

    You should not use any type of open flame at any point during this extraction. Use adequate ventilation at all times.

    Preparing your cactus

    You'll want to begin with dry powdered cactus if you can. You can dry slices of cactus in the oven with low heat and then use a coffee grinder to powderize it.

    NOTE: I've experience a severe reaction to breathing the powder. It screws up my sinuses for a week or two. I'd suggest using a face mask to prevent it being inhaled. Also I have noticed irritation to the eyes if the dust comes in contact with them. Be careful.

    Extracting

    Prepare a solution of lye water by slowly mixing together 1 TBS of lye for every pint(8 TBS/gallon) of cold water that you think you'll need to completely cover you dry cactus. This will produce a little heat so don't be alarmed. Just swirl it around slowly as you add the lye a little at a time. This is what I will refer to as base or basic water.

    Next add you dry cactus powder. Mix the contents thoroughly to ensure that you expose all of the powder to the basic water.

    Now add about a pint or so of xylene to the mix. You want enough of a layer to be able to draw off the xylene with the turkey baster later. Shake it all up and let it sit for an hour. This is what it will look like just after shaking.

    If after an hour you can see that the xylene layer is separating back out, fine, if not, add a little more pre-made basic water and check again. Now shake it back up and put it away for 24 hours (every second of it).
    This is after three hours.

    24 hours later, you want to draw off the xylene so now you need to use the turkey baster to suck it up and put it in a new jar(a mason jar works fine). You don't want any of the water from beneath the xylene to come with it. And put it into your salting bottles.

    Salting

    Now you want to mix your acid water in order to dilute it to the proper strength you want. Be very careful not to breath the vapors that come out of the bottle when you open it. HCL comes very strong and it will burn you.
    You want to add approximately 4-8 drops of HCL acid to 1.5 cups of water. Slowly add this acid water to the xylene while gently swirling the liquids around in the jar. Add just enough to make a half inch or so layer beneath the xylene.

    Don't worry that you won't get all of the goods because the xylene is going back into the extraction bottle and you'll get another shot at what you missed before. Put the lid on the jar and shake it all up. Wait a few minutes and shake again.

    Once it has returned completely to a separated state loosen the lid on the jar and place it in the freezer. You want the bottom layer(the acid water) to now freeze solid. The xylene will not freeze. Once the water is frozen, work quickly and pour the xylene back into the extraction bottle.

    With the water still frozen solid, pour in a little warm water and swirl around and discard quickly. This helps get rid of a little more residual xylene. The rest will evaporate later.

    Repeat the extraction and salting steps 4 to 6 times to get all of the goodies. You can reuse the xylene over and over again.

    Evaporating

    Now thaw out the water and put it in you evaporation dish. A large flat bottomed pyrex dish works best. Using heat(heating pad beneath the dish) or not, fan dry it to evaporate the water from the dish. This may take some time depending on how much water you used. Once all of this is dry you will see a crystalline residue left on the dish.

    This pic shows off a mistake that I made and one that some of you may make also. On the right side of the dish you can see a huge brown spot. This happened because I used too much hcl acid in the salting step. This, however, is not a big problem. It will all be gone after the cleaning step, plus much of it evaporated with the water. I might could have even avoided some of the discoloration by evaporating slower, giving the hcl more time evaporate. Scrape it off with a razor blade. Mescaline hcl will be a brownish powder.

    This is from the first scraping from the first salting. It actually turned out much better than I normally expect. It can be used as is but the next procedure is simple if you've got this far.

    Cleaning

    Put a cotton ball in the spout end of your funnel so that it can filter. Mix some acetone with your extracted alkaloids. I use a mason jar so that I can swirl it around easily. You want to get every piece of mescaline washed with acetone, so mix it in good.

    Next, pour it into the funnel with a clean dry jar to catch the liquids. Use acetone to wash loose needles, that remain in the jar, into the funnel.

    You will notice some color draining through with the acetone. Wash like this with fresh acetone until little to no more color is draining through. Put the funnel somewhere to dry.

    Once all acetone smell is gone from the funnel and it's contents you need to pour some hot water into it with it positioned over the evaporation dish. The hot water will dissolve the crystals and allow them to flow through the cotton into the dish.

    Evaporate as before. The resulting crystals will be considerably whiter and more pure. This is not only for aesthetics, but also it makes for more accurate dosing.

    You can put this powder in capsules to facilitate simple dosing with pre-measured amounts in each capsule.
    __________________
    "there is no need though to seek death-
    it will find us .
    seek instead to become a light in this dark world."
     
  12. ancient powers

    ancient powers Member

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    mescaline HCL crystal
    --------------------------------------------------------------------------------
    below is a dream i had i dont know what it means but it seemed so real maybe others have had similar dreams about stuff........................weird kind of colourful .....great dream should be a movie ...

    • A buchner vacuum flask with buchner cup and #101 or #103 filter disc paper.
    * A vacuum source for the above vacuum flask, be it an aspirator and faucet or a deluxe food saver or other
    dedicated vacuum source.
    * epsom salts
    * A sep funnel
    * lab hot plate
    * sand
    * cake plate
    * xylene
    * acetone
    * lye
    * measuring cup
    * jars
    * MEK (methyl ethyl ketone)
    * boiling stone
    * erlenmeyer flask
    * glass carboy & stopper
    * long glass pipette to siphon up xylene from carboy
    * distilled water
    * blender to chop up the cactus
    * empty alcohol HDPE bottle for the gasser
    * Calcium Chloride for the gasser
    * muriatic acid for the gasser
    * mip adapter for the gasser
    * hose for the gasser
    * home made fume hood
    * pyrex brownie dish
    * fan
    * refridgerator & freezer

    pieces of cactus are dried allready, then they are put into a blender and ground up to a fine powder.

    Then the powder is put in the glass carboy with 1.5 gallons of water.
    I've never had any emulsion problems...everything runs as smooth as glass.

    If you ever notice any "clumping" of cactus powder together, you just stick in a metal rod and poke at it for a few minutes, and the clump will seperate and the pieces will re-distribute. I noticed one clump in the beginning, but it broke it up in a few minutes, and all went fine after that.
    But I always prepare my lye water by adding 9 oz of lye to 1/2 to 1 pint of hot water very slowly with stirring...then when it's all good and mixed, I pour it into the carboy.

    Then I add about 40 ounces of xylene. Then the carboy gets rolled around on carpet pieces for a few minutes, and then left to sit upright undisturbed for 2 days...then I just pull off the top xylene layer, it seperates just fine.

    Summary:

    1) 2.5 to 3 gallon water jug (carboy) + 1.5 gallons water + 27 ounces of lye <mix> + 1 kg powdered torch + 48 ounces xylene <mix repeatedly then let sit 2 days> 27 ounces of lye = about 3 and 1/2 cups of lye 48 ounces xylene = about 1400 mL Mix your carboy by rolling it around on carpet or carpet pieces, back and forth for a few minutes, repeat this a few times during the better part of a day, then let it settle for 2 days at least.
    I ordered one of those 3 gallon glass carboys from a beer making supply place

    2) siphon about 40 to 44 ounces of the xylene off the top put into a vacant 1 quart (1000 mL or 1 liter) jar
    Use a long glass pipette and it will take you about 15 to 30 minutes to siphon off the top xylene layer .
    By using a glass pipette, you will experience no dribble or splashback of get away drops back into your carboy as you are pulling...very effective but takes some time.

    3) Add 8 to 9 ounces of lye to about 300 to 500mL of water in a jar, add very slowly with stirring...after it is all mixed, add it to your carboy using a funnel. I like to heat a jar half full of water in the microwave for 2 minutes,then take it out and place it on a cement floor and then add your 8 to 9 ounces of lye very very slowly to it with stirring so it mixes together faster. Wear gloves & safety glasses...it will bubble a little bit in the beginning...just pour the lye in VERY slowly. As the jar cools down, you will be able to add the lye a little bit faster.

    4) Now add 40 to 44 ounces (1100 to 1300mL or so) of fresh xylene to the carboy.

    5) Roll the carboy around on the carpet to mix everything up real good...roll the carboy around every now and then during the day, then let it sit for 2 days undisturbed (very important).

    6) Just pull off the top 40 ounces (1000mL) or so of the top xylene layer and put it into another 1 quart jar.

    7) Repeat this entire process two more times, each time adding 8 to 9 ounces of lye to your carboy and more xylene...
    In the end you will have four 1-quart jars full of xylene containing Mescaline freebase.

    9) Now just dry your jars Combine your 4 jars into 1 single large glass jug to dry if you want.

    10) Now just gas your jars Combine your 4 jars into 1 single large glass jug to gas if you want.

    11) Bubble air through each of your jars for 5 minutes to "bleed" off any excess hcl gas lingering in the xylene.

    Use an aquarium pump..connect the tubing to the narrow end of a glass pipette and insert the wide end of the pipette into the jar.

    12) Let the 4 jars sit for 1/2 hour, you will see a layer of Mescaline hcl collect on the bottom of each jar. Add the bottom containing xylene with the Mescaline hcl (decant off most of the top layer of xylene into a jar to dispose of) to your sep funnel.

    13) Add 1/4 to 1/2 cup or less of hot boiling distilled water to the sep funnel. Let it sit for 10 to 30 seconds or less...decant off the clear bottom water layer...it contains your Mescaline hcl. You can also "shoot" the hot water into the sep to have it forcefully penetrate the xylene by using a water bottle with tip. The faster you collect your Mescaline , the better.

    14) Put the water into a pyrex dish and put it in the oven for 30 minutes at 200 degrees F

    15) Pull the pyrex dish out and let it sit under a fan overnight.

    16) In the morning scrape up your Mescaline hcl and clean it with a 5 minute acetone wash, evaporate water overnight again, then scrape up the Mescaline hcl in the morning...it will be very clean now and ready for consumption in dreams.

    This is the ghetto handheld gasser

    Materials needed for the handheld ghetto gasser:
    #1 91% isopropyl alcohol HDPE 32 fl oz (946mL) bottle
    #2 Watts A-300A i.d. barb to mip adapter 3/8" by 1/2"
    #3 25' roll of watts polyethylene 1/2" by 3/8" tubing used for food/water cut off a short piece.
    #4 box (calcium chloride)
    #5 jug of 31.45% muriatic acid
    #6 measuring cup
    #7 gloves
    #8 gas mask
    #9 safety glasses
    #10 home made fume hood
    #11 funnel (for pouring the CaCL & muriatic into the bottle)

    DO NOT PROCEED WITHOUT READING THE FOLLOWING VERY CAREFULLY:
    The procedure described below is potentially very hazardous. It uses anhydrous hydrogen chloride gas to salt Mescaline instead of an aqueous solution. Hydrogen chloride gas is an extremely noxious and potentially deadly compound. The procedures described herein are safe as written, however, accidents are possible. Do not even think about attempting this method without first securing a suitable gas mask or organic vapor mask capable of filtering hydrogen chloride fumes. Learn how to use the mask ahead of time and wear it at all times while the apparatus described is in operation. Work only in well ventilated areas. Do not attempt this procedure in a house where children or invalids are present.

    Failure to follow all safety precautions can result is serious personal injury or death.

    Hydrogen chloride gas is serious business people. Don't fuck around with this. If you are unable or unwilling to follow the safety precautions, then you would be better off not using this method.

    All that being said, however, I believe the device shown below to be quite safe. It produces only small amounts of the gas as needed and anyone who can follow directions and has common sense can safely produce beautiful results with this method.

    HCL gas is dangerous. Do not breath it.

    This gasser produces small amounts of gas on demand by squeezing but you still must do this outside (still wearing your gas mask) or use it inside a fume hood. HCL gas will corrode metal stuff on contact, so keep it inside your fume hood. You must wear safety goggles, gloves, pants, and of course, the gas mask at all times when preparing the bottle and using it. But don't worry it is completely safe...this is even easier then the standard titration.

    Assemble the bottle, mip adapter & hose wand and practice "gassing" a jar of water with air to get a feel for how it operates. Each squeeze will let out 10 to 15 medium sized bubbles. Hold the "squeeze" while the wand is submerged and don't let go of the "squeeze" until you take it back out of the liquid.

    It's very easy to operate.
    Before beginning, make sure your fume hood is turned on and the fans are pumping air to the outside through the window. Make sure you are wearing jeans, safety glasses, gloves, and gas mask.
    Have 2 to 4 of your 1000mL or so xylene pull jars (pull #1 and pull #2 jars) sitting in the fume hood with the lids off. Or you can combine all your pulls into a single gallon or bigger jar to be gassed.
    #1) Add 500mL (2 cups) of Calcium Chloride to the empty alcohol bottle, then add 120 mL (1/2 cup) of muriatic acid to the bottle...you will see it bubble a tiny bit...screw on the barb adapter attachment. The barb adapter should have hose allready attached to it--no glue necessary--they fit perfectly together and will be extremely difficult to pull apart when together. The barb threads into the top of the bottle, perfect fit. Now just put the hand held gasser in the fume hood and let it sit for 2 minutes (wait for the cacl to do its thing and suck the water from the muriatic, leaving pure concentrated gas in the bottle). Now just pick up the gasser and press on it a little bit and you will see a "puff" of pure hcl gas exit the wand...do this a few times in the fume hood so you can make sure the fume hood is working really good...my fume hood has 6 brushless fans and immediately sucks any fumes in the hood and exits them out to the outside right away.
    #2) Now insert the wand into the jar #1 --1000mL or so of 1st xylene pull -- make absolutely sure you have dried the non-polar with Mescaline freebase through a filter of dried epson salts first to capture any water from the non-polar--it needs to be dry, dry, dry to be gassed and leave us with sparkly white Mescaline right away.
    Squeeze on the bottle while the wand is submerged in the non-polar, it will bubble about 10 to 15 medium sized gas bubbles, then pull wand out while still holding the "squeeze" on the bottle....Repeat this about 5 to 10 more times...this only takes a minute or two....you will immediately see a "snow" of Mescaline crystals form in the dried non-polar and they will sink to the bottom.
    #3) the recipe given above will produce enough gas to gas all four of the xylene pulls .
    #4) hook up the end of an medium power aquarium bubbler ($20 or so) to the narrow end of a long glass pippette and insert the pippette into each of the jars for 5 minutes to bubble air through the non-polar to "bleed" off any excess hcl gas that might be trapped in the non-polar--this will aid in case you decide you want to extract your mesc hcl off with water from the non-polar. It will keep your Mescaline pure white and not discolored by any excess hcl in the non-polar.
    be sure to bubble air thru each collection jar after gassing for about 5 to 15 minutes to evacuate off any lingering hcl gas. I used a pretty strong medium level aquarium pump, so I bubbled air for about 5 min. This will ensure your Mescaline pull will stay white/clear/off white when you pull it...so long as your non-polar was dried properly as well.
    IMPORTANT: when done gassing, screw the barb off the bottle, put the bottle under a sink faucet, and fill it up to the top with cold water to stop the reaction from producing gas inside the bottle. Then dispose of it properly.
    The bottle will be warm from the reaction and the water will also serve to cool it down. Don't worry--it doesn't get over 140 degrees.
    How did the gassing go? Did you find it easy?
    How many times did you submerge the wand in the non-polar and gas it?
    About 5 to 10 times?
    Also, you may find that you get a much cleaner product by using a sep funnel...pour your gassed xylene into the sep funnel, and allow the Mescaline to fall to the bottom over a period of 30 minutes...it will all collect at the bottom, from this point on you have 2 options:
    1) Option #1 is to collect with boiling hot water....pour your boiling hot water into the sep funnel, then it will collect on the bottom and pull your Mescaline out...drain it all out within 30 seconds or so, then put it into a pyrex brownie dish, evaporate off the water overnight, then scrape it up and clean it with an acetone wash.
    --------------------------------------------------------------------------------------------------------------------------------
    2) Option #2 will give you very clean product....pour your gassed xylene solution into the sep funnel, and wait 30 minutes for all the Mescaline to fall and collect at the bottom of the sep funnel.
    Then just drain out the bottom Mescaline layer
    Pour the jar into a sep funnel.
    Wait 30 minutes, and all of the yellow stained Mescaline hcl will collect at the bottom of the sep.
    Drain out the yellow stained Mescaline into a buchner cup with a filter disc and put it on a buchner funnel vacuum setup.
    Clean it with acetone and rinse with more acetone (at least 3 times)
    the yellow goo ball that drops out of the lower part of the sep funnel...after a while the xylene evaporates off the product, but as it's evaporating you can see white Mescaline oozing out of it and collecting on the dish.
    7.) The yellow goo ball must be cleaned and rinsed with acetone on a buchner cup Then you must use boiling hot water/acetone re-crystallization to drive off the solvent fumes from the white mescaline...this also gets it crystalline pure.
    Part I, Post Gassing Clean-up
    Filter the mescaline.hcl from the gassed xylene with a buchner funnel & vacuum. (or if you put it
    into a sep funnel, it will be the lower bright yellow layer, just drain it out into a small puddle). Wait a little white for the xylene to evaporate off the powder.
    Then wash the powder with clean xylene. This flushes through any brown cactus crap that was
    also in the xylene.
    Now disconnect the vacuum hose to break the vacuum. Then reattach it, but leave the vacuum
    turned off. This creates a sealed volume of air, so when you pour liquid on top of the filter paper,the trapped air will tend to keep it there instead of allowing it to drain through.
    Now using a wash bottle, wash the powder with acetone until it's completely covered, and let it
    sit for a couple of minutes. Then turn the vacuum on, and filter through the acetone. Now rinse
    the powder with more acetone as it's being sucked through. This soaking and washing will remove the vast majority of the xylene.
    Cover the filter funnel with a large oversized piece of filter paper, and suck air through the funnel for a couple of minutes, this will help dry the powder and protect it from dust.
    Now remove the filter funnel and allow the white powder to completely dry.
    This entire procedure on pull jars #3 and #4 from a cactus carboy tek took only about an
    hour and a half. Most of the time was spent taking pics. I decided to pull the Mescaline hcl out of the gassed jars with water in a sep funnel, as I didn't want to loose any Mescaline to the filtering process...last time I lost about 1 gram of Mescaline hcl to the #103 2.5 micron filter disc even though it collected about 4 grams on top. I then collected the 1 gram that got thru the filter disc with a sep funnel and water.
    If you decide to collect with filtering and vacuum buchner instead, be sure to wash the heck out of the Mescaline several times (3 to 4 times) with acetone and rinse it liberally.
    You just have to experiment using the 2 collection methods, and find which one you like best. I like using a sep funnel, 1/2 cup of boililing hot water (the traditional way) the best. Don't worry your water is neutral and not acidic so it won't pull out other cactus ca-ca like a typical xtraction can do.
    at the end of gassing the jars, the handheld ghetto gasser does get warm, but it doesn't get all that hot.
    I submerged the wand and squeezed it to make bubbles anywhere from 5 to 10 times for each jar. At the end of the gassing which only took a minute or too, water from a nearby gallon of water was poured into the bottle with a funnel to extinguish it. After a while, the Calcium Chloride will turn rock hard at the bottom and won't come out. Fill the bottle all the way to the top with water when you are done, screw on the lid and put it into a single black garbage bag and dispose of it properly along with your normal trash.
    It is so easy to use...it doesn't puff out gas until you need it--by holding the gasser and giving it a gentle squeeze, you will then see about a 4 to 5 inch puff of gas (when it reacts with the moisture in the air, it can be seen). It does not exit gas continuously like a locomotive or anything, it's only available when you need it,so it's very safe. If for some reason you need more gas, just swirl or shake the bottle a little bit...but I didn't have to do that at all...it made plenty of gas and exited the gas on demand just by squeezing...Even after gassing the 2 jars, it still was able to put out more gas easily by squeezing on it...this was all done inside of
    a fumehood. The fumehood was put in front of an open back window
    the dried epsom salts after they were used -- they turn yellow after sitting in the xylene. Rinse your now yellow salts and filter disc with fresh xylene through a 2nd fresh #101 filter put on the buchner cup again to top off the jar. This will collect any lingering non-polar from the salts and filter you used.
    Concerning the re-crystallization:
    You should always do an acetone wash on your stuff no matter how good it looks. I've ALWAYS had excellent trips (over a dozen now) from acetone washed mescaline...my favorite.
    1) Just put your Mescaline from the scraped up pyrex dish into a mortar & pestal, add ice cold acetone, and pestal it for a few minutes real good, this will "scrub" the crystals clean.
    2) Put a cotton ball into a funnel mounted on your vacuum flask and pour your mixture from the mortar & pestal through it.
    3) Turn on the vacuume and vacuume it for a few seconds to pull out any trapped acetone from the cotton.
    4) Pull the cotton out of the funnel, and put it under a heater/fan to dry...this may take a few hours...make sure it is absolutely dry before going to the next step.
    5) In a few hours when the cotton is all dry, I'll put it back into a clean funnel, then pour boiling hot water thru the funnel & cotton, collect the hot water that falls thru on a pyrex dish, then evaporate off the water under a heater/fan to re-collect the now cleaned up mescaline.
    The bright yellow color washes away from the gassed product VERY EASILY and QUICKLY with acetone as you can tell. The product is indeed white, but it is not done yet! It needs to be added to boiling hot water to drive off any solvent fumes--this will eliminate all chemical residue, taste and smell from the product.
    Just follow boiling hot water/acetone re-crystallization above or another method of re-crystallization of your choosing.
    THE ULTIMATE COMPILATION OF DUAL and TRIPLE SOLVENT RE-CRYSTALLIZATION METHODS for Mescaline hcl :
    I'm going to list and describe all the details of 4 popular methods below...also don't forget the 5th method above
    Study and pick the re-crystallization method you like the most....experiment till you find the one you like the best. Once you read all the methods in this post, you will see how similar they are and have a better overall understanding of re-crystallization.

    Refer to Chapter 13 "Recrystallization" pages 119 to 133 for an excellent description of how to re-crystallize with pictures from the book The Organic Chem Lab Survival Manual by James W. Zubrick.
    You will need a lab hot plate or similar (no flames), your solvent and product, and an Erlenmeyer flask, not a beaker. "If you recrystallize compounds in beakers, you may find the solid climbing the walls of the beaker to get at you as a reminder. A 125ml Erlenmeyer usually works."
    HOW TO RE-CRYSTALLIZE:
    EXPLANATION:
    The MEK (methyl ethyl ketone) thing is a dual solvent recrystallization: MEK and water. The impurities are soluble in both water and MEK, but are slightly more soluble in MEK then the Mescaline is. That's why the Mescaline will drop out first.
    This has to be done quite precisely because if you add too much water, then not all your Mescaline will precipitate out. But if you don't add enough water, then the impurities stay stuck to Mescaline powder instead of dissolving into the solution. So you have to use well dried MEK, and once it's boiling, you add 1 drop of water at a time, just until all the Mescaline powder dissolves. This gets both the impurities and the Mescaline dissolved in the MEK/water mix. And then the solution becomes clear instead of shimmery. It would help if you could stir the solution with a glass rod in between water drop additions, as this helps get everything mixed
    round well, and would help to avoid adding too much water.
    After getting the Mescaline powder to dissolve, you boil the solution to drive off the water (along with some of the MEK) until the solution becomes saturated (shimmery again). The loss of some of the water is what makes some of the Mescaline precipitates out as tiny seed crystals. When the solution is cooled down, the rest of the Mescaline grows on those crystals, forming large ones. The impurities stay in the solution.
    THE PROCESS:
    Put 3 grams sanchez in erlenmeyer flask with 150 mL boiling mek (a large excess of mek.) Use around 50 mL per 1 gram of sanchez. Put a boiling stone or chipped piece of porcelain in your flask too. Add water drop by drop until all the Mescaline dissolves, it will go from a "cloudy" appearance to a "clear" appearance when you have added enough drops of water, this means the last of the Mescaline has dissolved. You can stir it a little with a glass rod after each water drop addition to make sure it mixes in well. If your lab hotplate has a built in stirrer, then you can turn on the stirrer for a while after each addition. Then just boil down until the liquid begins to "shimmer" --- it will take on a shiny shimmering appearance. Stick it in the freezer for a couple of hours. If no crystals appear, simply boil it some more and shove it back in the freezer. Once you have crystals, simply filter them off and rinse with cold very anhydrous acetone. Let dry.
    Add crystals to a minimal amount of boiling hot water in a pyrex brownie dish sitting under a fan to drive off any acetone fumes...When water has evaporated, scrape up the crystals. Eat crystals. Trip balls.
    Make sure you use a laboratory style hot plate with a thin skillet or cake plate of sand with or without added mineral oil added to the sand, or an aluminum cup with mineral oil bath to hold your flask...and a fume hood is a must if this is being done inside.

    Keep a fire extinguisher on hand, baking soda, a bucket of sand, wet towel, etc. for safety reasons. Don't have any open flames anywhere, not even a pilot light, and don't smoke. Wear full protective goggles, heat resistant chemical gloves, long sleeve shirt.

    For really big crystals, put the flask in a pot of boiling water that has been taken off the stove and put on a mitten on a table, cover the top of the flask...the pot will take ages to cool down...this will help develop awesome crystals, then when the pot reaches room temp, put your flask in the refridgerator, then move it to the freezer overnight. In the morning you will have tons of beautiful pure white to see-thru transparent crystals depending on how clean your stuff was to start with. The gassing gives you pretty clean stuff anyways, see post #54 for
    typical color of post gassed product. Your MEK will be brown to gold colored...just filter off your crystals over a #101 to #103 round disc filter sitting in the buchner cup of your vacuum filter flask and rinse them with ice cold anahydrous (dried) acetone.
    To make the acetone anahydrous (remove the water) bake a thin layer of epsom salts in the oven at high temp 400 degrees F. for a couple hours. They will turn white. When it cools down crush it up a little, use a spatula to scrape it up. Throw a few hand fulls in your tin of acetone. Leave it for an hour or two and shake it every few minutes. Decant off the top layer of acetone above the rocks and filter it a few times thru a #103 filter disc on a vacuum flask before you use any. If your acetone is anahydrous you won't loose any product when you rinse the
    crystals.
    Materials list:
    * Ring stand
    * Stainless steel mixing bowl to hold the water bath on the hotplate/stirrer
    * Buret clamp (should have rubber jaws to hold grip on the flask, I don't like metal touching glass, or you can wrap plumbers tape around the jaws or the neck of the flask.) It's easy to find buret clamps with rubber coated jaws for about $7.
    * 125 to 250 ML erlenmeyer flask
    * distilled water and pipette to "dropper the drops of water in"* 150 ML of pre-dried MEK (dry the mek in the can with dried epsom salts, decant off the top portion of the MEK above the rocks and then filter it thru a #103 filter disc)
    * 3 grams of non-pure or dirty mescaline
    * boiling stones (alumina or teflon typical boiling stones)
    * hotplate with built in magnetic stirrer
    * stir bar
    * home made fume hood
    * open back window
    * electronic temperature probe/thermometer (about $12 from dept store, kitchen section), not necessary but handy to measure temp of the water bath.
    * fridge and freezer - allow the slow growth of large crystals, move your post-boiled MEK to room temp, then to fridge, then to freezer overnight for the best largest crystal growth.
    * fire extinguisher (for safety reasons on standby, can never be too safe)
    * sand/wet towel (on standby for safety reasons, can never be too safe)
    * safety goggles and gloves
    * remember no open flames, no lit pilot lights, no smoking.

    The flask shouldn't be touching the bottom of the bowl. It does matter, because if it is touching, then the bottom of the flask will heat up hotter then the rest of the flask. This creates a heat gradient which stresses the glass,it's not as bad as just plucking it on a hot plate, but it's not good for it, and it's more likely to bump. Bumping is when the bottom of the liquid heats up hotter then the top, and then it super boils spraying stuff all over.Constant stirring, or boiling stones help stop this, but bumping is minimized by using a water or oil bath, rather
    then putting it on the heating element.
     
  13. ancient powers

    ancient powers Member

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    3
    LSD Directly From The Lysergic Amides — The One-Pot Shot

    When the lysergic amides have been extracted in pure form from the crop, work should begin without delay to convert it to LSD. Diligence in this matter is very important because possession of the extracted amides is strong evidence of intent to manufacture LSD. Further, mere possession of lysergic acid or ergine is prohibited as they are federal "controlled substances." The goal must be to get the hot potato out of one's hands and convert it to cash as fast as possible. There are several possible methods to follow in the conversion of the lysergic amides to LSD. The first two presented in this book are excellent, and highly recommended. The third one is OK. Beyond
    that, we are talking last resort. In all cases, the overriding factor which
    must take precedence is ease of availability of the required chemicals. A
    bottle of trifluoroacetic anhydride in hand beats homemade anhydrous hydrazine in the bush.

    The first LSD manufacture method presented here is what I like to call "the one-pot shot." It can be found in US patent 3,239,530 and US patent 3,085,092, both granted to Albert Hofmann. This method uses anhydrous hydrazine to cleave the ergot amides to produce lysergic acid hydrazide. The hydrazide is then isolated by extraction, and reacted with acetylacetone (2,4-pentanedione) to form a pyrazole intermediate, which is then reacted with diethylamine to form LSD. This method at first glance seems complicated, but the actual manipulations involved here are less challenging than proceeding through lysergic acid. Further, the yields are higher with this method than those proceeding through lysergic acid, and there is less
    formation of the inactive iso-LSD than with other methods. Iso-LSD is
    not a complete loss since it can be converted to the active LSD, but it is
    best to avoid its formation in the first place.

    This method has a serious drawback. Anhydrous hydrazine is not available off the shelf at your local hardware store, and attempts to procure it through normal channels are likely to catch the attention of those shit-eating dogs at the DBA. I include in this chapter directions for making your own anhydrous hydrazine, but be warned here that failure to use a nitrogen atmosphere during the distillation of anhydrous hydrazine will likely lead to an explosion. On that cheery note, let's begin!

    Step One: Conversion of Ergot Amides to Lysergic Acid Hvdrazide

    The reaction above is illustrated for ergotamine, but the process is just as valid when a mixture of amides is used as extracted from the crop. Further, the crop amides have been left in the freebase form, so the procedure given in example 5 in US patent 3,239,530 is used. This is superior to trying to make a hydrochloride salt of the amides, as suggested in example 1, because this would expose the active ingredients to loss and destruction during the unnecessary handling.

    There are three main precautions to be followed while executing this procedure. Water must be rigorously excluded from the reaction mixture, as hydrazine hydrate will react with the amides to form racemic lysergic acid hydrazide rather than our desired product. To ensure the exclusion of water from the reaction, the glassware should be baked in an electric oven prior to use, and be allowed to cool off in a dessicator. A drying tube should be attached to the top of the condenser used, to prevent humidity in the air from getting in the mix.

    Naturally, the hydrazine used had better be anhydrous. Another danger to success is exposure to light. Work should be done under a dim red darkroom bulb. The flask containing the reaction mixture should be wrapped in aluminum foil to exclude light. Procedures such as extractions and filtering should be done as rapidly as possible without causing spills. Finally, this reaction should be done under a nitrogen atmosphere, as hot hydrazine and oxygen do not get along too well.

    In a 500 ml round-bottom flask place a magnetic stirring bar, 10 grams of the ergot amide mixture (dried in a vacuum dessicator to ensure its freedom from water), 50 ml of anhydrous hydrazine, and 10 ml of glacial acetic acid. A condenser equipped with a drying tube is then attached to the flask, and the flask wrapped in a single layer of aluminum foil. The flask is then lowered into a glass dish containing cooking oil heated to 140° C on a magnetic-stirrer hot-plate. When the flask goes into the oil, the heat should be backed off on the hot-plate so that both oil and flask meet each other in the middle at 120° C.

    Monitor the warming of the contents of the flask by occasional insertion of a thermometer. Stir at moderate speed. In about 10 minutes, the desired temperature range is reached, and some gentle boiling begins. Maintain the temperature of the oil bath at 120-125° C, and heat the batch for 30 minutes.

    When 30 minutes heating at 120° C is complete, add 200 ml water to the batch, increase the oil temperature to 140° C, and rig the glassware for simple distillation. Distill off between 200 to 250 ml water, hydrazine hydrate and acetic acid mixture. Then remove the flask from the heated oil, and allow it to cool. Use of an aspirator vacuum to assist the distillation is highly recommended.

    When the flask has cooled, add 100 ml of decimolar tartaric-acid solution (1.5 grams tartaric acid in 100 ml water) to the flask, and 100 ml ether. Stopper the flask, and shake vigorously for a few minutes, with frequent breaks to vent off built-up pressure from the flask. If the stirring bar bangs too violently in the flask, remove it with a magnet rather than break the flask.

    Pour the contents of the flask into a 250 ml sep funnel, and drain the lower layer (water solution of lysergic acid hydrazide tartarate) into a 250 ml Erlenmeyer flask wrapped in foil. To the ether layer still in the sep funnel, add 50 ml fresh decimolar tartaric-acid solution, and shake. Examine the water layer for the presence of lysergic acid hydrazide with a black light. If there is a significant amount, add this also to the Erlenmeyer flask. Place the magnetic stirring bar in the Erlenmeyer flask, and stir it moderately. Monitor the pH of the solution with a properly calibrated pH meter, and slowly add .5M (20 grams per liter) sodium hydroxide solution until the pH has risen to the range of 8-8.5. Higher pH will cause racemization. The freebase is then extracted from the water solution with chloroform. Two extractions with 100 ml of chloroform should complete the extraction, but check a third extraction with the black light to ensure that most all of the product lysergic acid hydrazide has been extracted.

    The chloroform extracts should be evaporated under a vacuum in a 500 ml flask to yield the product. This is best done by rigging the 500 ml flask for simple distillation, and applying an aspirator vacuum to remove the chloroform. Assume that the yield from this procedure will be about 5 grams of lysergic acid hydrazide if ergot was the crop used. Assume that the yield will be about 7.5 grams if seeds were used. The difference here is due to the fact that in ergot, the amides are largely composed of substances in which the portion lopped off is about as large as the lysergic acid molecule. Seeds tend to be more conservative as to their building upon the lysergic molecule. A careful weighing on a sensitive scale comparing the weight of the flask before and after would give a more exact number.

    Both of these choices are really very poor, because lysergic acid hydrazide, unlike most other lysergic compounds, crystallizes very well with negligible loss of product. At the hydrazide stage of LSD manufacture, one has a perfect opportunity to get an exceedingly pure product, freed from clavine alkaloids and other garbage compounds carried in from the extraction of the complex plant material.

    I refer the reader to US patent 2,090,429 issued to Albert Hofmann and Arthur Stoll, the dynamic duo of lysergic chemistry, dealing with lysergic acid hydrazide. In this patent, they describe in a rather excited state how they were able to produce pure lysergic acid hydrazide from tank scrapings that were otherwise impure junk.

    Lysergic acid hydrazide has the following properties: it dissolves easily in acid, but is very difficultly soluble in water, ether, benzene and chloroform. In hot absolute ethanol it is slightly soluble, and is crystallizable in this solvent to yield "beautiful, compact, clear, on six-sided cut-crystal plates that melt with decomposition at 235-240° C." This is obviously the way to go. The hydrazide should be recrystallized from absolute ethanol, and then dried under a vacuum to remove residual alcohol clinging to the crystals. About 300 ml of hot ethanol is required to dissolve each gram of lysergic acid hydrazide during the crystallization. Upon cooling, a first crop of pure lysergic acid hydrazide is obtained. Then, by boiling away half of the mother
    liquor and cooling, an additional crop is obtained. This process can be
    continued as long as the crystals obtained look nice.

    Step Two: Lysergic Acid Pyrazole

    In this reaction, one mole of lysergic acid hydrazide is dissolved in an inert, water-miscible solvent like ethanol. Then an excess of 1-molar hydrochloric acid is added to form a salt with the lysergic acid hydrazide. To this mixture is then added two moles of acetylacetone (2,4-pentanedione), which forms the desired pyrazole. This reaction is not nearly as touchy as the formation of the hydrazide. The presence of traces of moisture from the air poses no problem. 2,4-pentanedione finds use in analytical chemistry as a chelating agent for transition metals, and as such should be available without raising too many red flags.

    Synthesis of this compound is not hard, and directions for doing so are found in US Patents 2,737,528 and 2,834,811.To do the reaction, the flask containing the 5 grams of hydrazide is wrapped in a single layer of foil to exclude light. Then a magnetic stirring bar is added, along with 18 ml of ethanol, 18 ml water, 20 ml 1molar HC1 (made by adding one part 37% HC1 to 11 parts water) and this mixture is stirred for a few minutes. Then 3.5 grams (3.5 ml) of 2,4-pentanedione is added at room temperature, and the stirring continued for an hour or so.

    The product is recovered from solution by the slow addition with stirring of 20 ml 1-molar NaOH (40 grams per liter). This neutralization throws the pyrazole out of solution as a solid. The solid is collected by filtration through a Buchner funnel, and rinsed off with some water. The crystals are then dried under a vacuum, preferably with the temperature elevated to 60° C. Further purification can be done by crystallization. If so desired, dissolve the crystals in chloroform, then add 8-10 volumes of ether to precipitate the product. I do not feel this is necessary if the hydrazide used was reasonably
    pure, since all the reagents used in the last step are soluble in water.The water rinse should have carried them away. Further, alcohol and
    2,4-pentanedione are volatile, and would be removed in the vacuum drying.

    Step Three: LSD

    This simple and easy reaction is done as follows: In a flask wrapped in a single layer of foil are placed 1 gram lysergic acid pyrazole, and 30 ml diethylamine. Diethylamine is a definite "do not purchase" item. Easy directions for its synthesis are given in this chapter. The two ingredients are swirled until mixed, then allowed to stand at room temperature for about a day.

    The excess diethylamine is then distilled off, and saved for use in future batches. Dimethylpyrazole is a high-boiling-point substance, and easily separated from diethylamine. When most of the diethylamine has been distilled off, a vacuum is applied, and the residue is evaporated to dryness. The evaporation is completed by warming the flask in boiling water for a few minutes with continued application of vacuum. The residue is almost pure LSD.

    Purification and Storage

    At this point, the process has yielded LSD freebase. In this state, the substance is quite unstable and not suitable for storage. A judgment as to the purity of the product is therefore needed in quick order, because which method of further processing to use is dependent upon the purity of the product. If there is reason to believe that a significant amount of iso-LSD is mixed in with the product, the following chromatographic separation is called for. The iso-LSD can then be recovered and converted to the active LSD, which greatly increases the value of the product. Iso-LSD can be expected to be formed using the process in this chapter if the additions of sodium
    hydroxide were not sufficiently slow, and local areas of high pH developed in the solution. Using methods in other chapters proceeding through lysergic acid, a large amount of the iso product can be expected if lysergic acid was made by use of hydrazine hydrate or HOH.

    Also, some of the natural alkaloids are of the iso form and yield iso-LSD. The procedure for acid production using trifluoroacetic anhydride will always make a lot of the iso product. The best procedure I can recommend is: whatever method has been used, check the product throughchromatography for the presence of the iso-LSD. The following procedure is taken from US patent 2,736,728.

    3.5 grams of LSD freebase is dissolved in 160 ml of a 3-1 mixture of benzene and chloroform (120 ml benzene, 40 ml chloroform). Next, a chromatography column is constructed from a burette. It must hold about 240 grams of basic alumina (not acidic alumina), so a 100 ml burette is called for. A wad of cotton and filter paper is stuffed down the burette against the stopcock to keep the particles of alumina from flowing out. The 240 grams of basic alumina are then poured into the burette with tapping to assure it is well packed. The alumina should then be wetted with some 3-1 benzene-chloroform.

    Now the 160 ml of benzene-chloroform containing the LSD is run slowly into the burette, followed by more benzene-chloroform to develop the chromatogram. As the mixture flows downward through the alumina, two zones that fluoresce blue can be spotted by illumination with a black light. The faster-moving zone contains LSD, while the slower-moving zone is iso-LSD.

    When the zone containing LSD reaches the spigot of the burette, it should be collected in a separate flask. About 3000 ml of the 3-1 benzene-chloroform is required to get the LSD moved down the chromatography column, and finally eluted. The iso-LSD is then flushed from the column by switching the solvent being fed into the top of the column to chloroform.

    This material is collected in a separate flask, and the solvent removed
    under a vacuum. The residue is iso-LSD, and should be stored in the freezer until conversion to LSD is undertaken. Directions for this are also given in this chapter.

    For the fraction containing the LSD, conversion to LSD tartrate must be done to make it water soluble, improve its keeping characteristics, and to allow crystallization. Tartaric acid has the ability to react with two molecules of LSD. Use, then, of a 50% excess of tartaric acid dictates the use of about 1 gram of tartaric acid to 3 grams of LSD. The three grams of LSD would be expected from a well-done batch out of a total 3.5 LSD/iso-LSD mix.

    The crystalline tartrate is made by dissolving one gram of tartaric acid in a few mis of methanol, and adding this acid solution to the benzene-chloroform elute from the chromatography column. Evaporation of the solvent to a low volume under a vacuum gives crystalline LSD tartrate. Crystals are often difficult to obtain. Instead, an oil may result due to the presence of impurities. This is not cause for alarm; the oil is still likely 90%+ pure. It should be bottled up in dark glass, preferably under a nitrogen atmosphere, and kept in a freezer until moved.

    If chromatography reveals that one's chosen cooking method produces little of the iso products, then the production of the tartrate salt and crystallization is simplified. The residue obtained at the end of the batch is dissolved in a minimum amount of methanol. To this is then added tartaric acid. The same amount is added as above: one gram tartaric acid to three grams LSD. Next, ether is slowly added with vigorous stirring until a precipitate begins to form. The stoppered flask is then put in the freezer overnight to complete the precipitation. After filtering or centrifuging to isolate the product, it is transferred to a dark bottle, preferably under nitrogen, and kept in the freezer until moved.

    LSD from Iso-LSD

    Two variations on this procedure will be presented here. The first is the method of Smith and Timmis from The Journal of the Chemistry Society Volume 139, H pages 1168-1169 (1936). The other is found in US patent 2,736,728. Both use the action of a strong hydroxide solution to convert iso material into a mixture that contains active and iso material. At equilibrium, the mixture contains about 2/3 active material and 1/3 iso material. These substances are separated by chromatography, and the iso material saved to be added to the batch the next time isomerization is done. In this way, eventually all of the product becomes active material.

    Method One

    The iso-LSD as eluted from the chromatography column is first evaporated under a vacuum to remove the solvent. The residue is then dissolved in 1-molar alcoholic KOH, and boiled under reflux, preferably with a nitrogen atmosphere, for 30 minutes. The mixture is next cooled and diluted with 3 volumes of water. It is next acidified with HC1, then made alkaline again with sodium carbonate. The product is now extracted from solution with ether or
    chloroform. After removal of the solvent, the product can be chromatographed as previously described.

    Method Two

    The iso-LSD as eluted from the chromatography is first evaporated under a vacuum to remove the solvent. The residue is dissolved in the minimum amount of alcohol, and then one half volume of 4-molar KOH in 100 proof vodka is added. The mixture is allowed to sit at room temperature for a couple of hours, then the alkali is neutralized by adding dry ice. The solvents are next removed under a vacuum, and the residue chromatographed as previously described.

    Preparation of Anhydrous Hydrazine

    Anhydrous hydrazine can be made from the easily available raw materials: bleach, ammonia, sulfuric acid and potassium hydroxide. This is not a task to be undertaken lightly, as there are dangers inherent in the process. Hydrazine will likely detonate during distillation if the distillation is not done in a nitrogen atmosphere. Also, hydrazine is a vicious poison prone to absorption through the skin or by inhalation of its vapors. It is very corrosive to living tissue, and its burning effects may be delayed. Hydrazine can also be assumed to be a carcinogen. All steps in its preparation must be done
    with proper ventilation, and protection of the body from spills.

    Step One: Hydrazine Sulfate

    2NH3
    + NaOCI ——> NH2 NH2 + H2O + NaCI NH2NH2
    + H2S04 ——> NH2NH2H2S04

    Into a 3-quart-capacity glass baking dish (Pyrex) put 750 ml strong ammonia (28% NH3), 350 ml distilled water, 190 ml 10% gelatine solution, and 700 ml 12.5% bleach. This strength of bleach is available from pool supply companies and makers of cleaners. The 5.25% strength Clorox will not do here. One must also be aware that traces of iron and copper have a very bad effect upon the yield, so do not dispense with the use of distilled water. The bleach is another possible source of iron. In checking out this reaction, the Pro Chemicals brand of bleach worked fine. I can't vouch for other
    brands. If all else fails, the bleach can be made from chlorine and NaOH in distilled water. (See Organic Syntheses Collective Volume 1, page 309.) The Pro Chemicals brand of bleach analyzed at 10 ppm iron by atomic absorption, and this amount did not interfere with the reaction. One must also check the bleach to make sure it is alkaline, as free chlorine prevents the formation of hydrazine.

    When the ingredients have been mixed in the baking dish, it is heated as rapidly as possible until it has been boiled down to one-third of its original volume. Being a wimp and boiling it down too slowly reduces the yield. Take not more than two hours.

    The dish is then removed from the heat, and allowed to cool. When the dish nears room temperature, it should be nestled in ice to chill thoroughly. The solution should then be filtered to remove suspended particles from the solution. The filtered solution is next put in a beaker, and nestled in ice mixed with salt until the temperature of the solution reaches 0 C.

    When that temperature is reached, 10 ml of concentrated sulfuric acid for each 100 ml of solution is slowly added with constant stirring. If the stirring is not strong, or if the filtering was poorly done, a product contaminated with brown particles results. If done well, hydrazine sulfate precipitates as white crystals. The mixture is allowed to stand in the cold for a few hours to complete the precipitation. The crystals are then filtered by suction, and the crystals rinsed off with cold alcohol. The yield is 25 to 30 grams of hydrazine sulfate.

    Step Two: Hydrazine Hydrate

    Mix 100 grams dry hydrazine sulfate with 100 grams powdered KOH and place the mixture into a copper and silver retort. Then add 15 ml water, and distill off the hydrazine hydrate formed though a downward-inclined glass condenser. There is little need for heat to be applied at the beginning of the distillation because so much heat is generated in the reaction between the KOH and the sulfate. Later, strong heating is required to distill out the last of the hydrazine hydrate.

    This crude product contains water beyond the monohydration of hydrazine. It is purified by fractional distillation. Pure hydrazine hydrate boils at 117° C to 119° C. The forerun contains the excess water. It should be converted back to hydrazine sulfate by addition of sulfuric acid as done in step one. The yield is 10 grams of hydrazine hydrate.

    During the fractional distillation, there are some precautions which should be followed. Hydrazine hydrate attacks rubber and cork, so the use of these materials must be avoided in the distillation. It also attacks most kinds of stopcock grease. The distillation is most safely done under nitrogen. Nitrogen should be introduced into the distilling flask, and the system flushed of air for about 15 minutes. Then the rate of nitrogen flow is reduced, and distillation commenced. The product will also attack glass, albeit slowly. It should be stored in 304 or 347 stainless steel. 316 stainless is not acceptable.

    Step Three: Anhydrous Hydrazine


    100 grams (100 ml) of hydrazine hydrate is mixed with 140 grams powdered sodium hydroxide. The apparatus is thoroughly flushed with nitrogen, then the rate of nitrogen addition to the distilling flask is slowed, and fractional distillation is commenced through an efficient fractionating column of about 15 theoretical plates. Anhydrous hydrazine distills at 112° C to 114° C. Anhydrous hydrazine is obtained at 99%+ purity.

    Another method for producing anhydrous hydrazine exists which gives a higher yield of product, but it uses anhydrous ammonia and more complicated glassware and procedures. See Journal of the American Chemical Society Volume 73, page 1619 (1951), and Volume 76, page 3914 (1954). Also see Hydrazine by C.C. Clark, The Chemistry of Hydrazine by L.F. Audrieth, and Industrial and Engineering Chemistry Volume 45, pages 2608 and 2612 (1953). Also see Inorganic Syntheses Volume 1, page 90 (1939).
    Anhydrous hydrazine can be stored in dark glass bottles under refrigeration for years.

    Other variations on the alkali hydroxide dehydration of hydrazine hydrate exist which give higher yields of less-pure hydrazine. See pages 48-54 in the Chemistry of Hydrazine mentioned above. It lists many references. Especially interesting is Journal of the American Chemical Society Volume 71, pages 1644-47 (1949).

    Preparation of Diethvlamine

    NH3 + CH3CH2I —s> xHI + CH3CH2NH2
    + (CH3CH2)2NH +
    (CH3CH2)3N

    The reaction which produces diethylamine also yields as by-products ethylamine and triethylamine. The relative amounts of each compound produced depends upon the molar ratio of the two starting materials. Use of only a little ethyl iodide favors the formation of mostly ethylamine. Use of a lot of the ethyl iodide favors the formation of triethylamine. Somewhere in the middle, a roughly even split occurs. This will be done here. See Journal of the American Chemical Society Volume 69, pages 836 to 838 (1947).

    A section of clean steel pipe 2l/2 to 3 inches in diameter is obtained, and fine threads are cut into each end so that a cap may be screwed onto each end. A really nice touch would be to have all the pieces plated with a half-thousandths-inch of electroless nickel, but the plater may think you are constructing a pipe bomb when he sees the pipe and caps.

    The bottom of the pipe is secured by screwing the cap on over threads coated with Teflon tape. Welding may also be used. The pipe is then nestled into a Styrofoam cooler, and is then filled about 1/2 full of rubbing alcohol, and then to this solvent dry ice is added, slowly at first to prevent it from boiling over, then more rapidly. The top of the pipe should be covered to prevent frost from forming inside the pipe as it cools down.

    Next, add 175 ml of ethyl iodide to the pipe, and let it cool down. It
    will not freeze, as its melting point is about 100° below O° C. Then liquid
    ammonia is added to the pipe. This is best done by inverting a cylinder of liquid ammonia, attaching plastic tubing to the valve, and cracking open the valve to feed the liquid into the pipe. About 525 ml of liquid ammonia is called for. In a 3-inch-diameter pipe, that plus the ethyl iodide will fill it half full. This is not an operation to be done in a residential neighborhood, as the fumes are tremendous. A rural setting with beaucoup ventilation is more proper.

    Now secure the top of the pipe by screwing on the cap tightly over Teflon tape. The pipe is now moved into a tub of ice water, and allowed to sit in this ice water for 45 minutes to an hour to warm up to 0 ° C.

    When the pipe has warmed to O° C, it should be shaken to mix the two reactants, and returned to the ice water. This shaking should be repeated a few times at 5-minute intervals. When 30 minutes have passed from the first shaking, the pipe should be returned to the dry ice bath and allowed to cool.

    When the pipe has cooled, the cap on the top of the pipe is loosened. Then the pipe is returned to the tub of ice water, and the ammonia is allowed to slowly evaporate away. This will take overnight, and raise great plumes of stink.

    After most of the ammonia has evaporated, the contents of the pipe should be emptied into a beaker. The foul substance is a mixture of ammonia, ethlyamine, diethylamine, triethylamine, and the hydriodides thereof. The best route to follow is to cool this mixture in ice, and slowly add with stirring 90 grams of sodium hydroxide dissolved in 100 ml of water. This neutralizes the HI in the mix, yielding the freebases of all.

    This mixture should be extracted several times with toluene. Toluene is chosen because it is available at the hardware store, and its boiling point is higher than any of the amines. The extracts should be filtered, and dried over sodium hydroxide pellets.

    The toluene extracts should then be transferred to a flask, and the mixture fractionally distilled through an efficient column. Ethylamine distills at 16° C, diethylamine distills at 55° C, and triethlyamine distills at 89° C. The diethylamine fraction should be collected over a 20-degree range centered on 55° C, and this fraction then redistilled to get the pure product. The yield of diethylamine is about 40 ml. Absolute freedom from water in the product can be assured by letting the crude distillate sit over a few chips of KOH for a few hours prior to the final distillation.

    Preparation of Tartaric Acid

    My experience with the chemical scrutinizers while ordering a pound of Rochelle salts should serve as a lesson to those embarking upon LSD manufacture. Substances which are useful for this purpose will raise red flags if obtained through normal channels. It must then be the highest priority to avoid these normal channels, or to subvert their scrutiny by preparing yourself those substances with direct use in the synthesis.

    The most low-profile method for getting tartaric acid is to follow the procedure given below. It uses cream of tartar from the grocery store and gives good results. See Chemical Engineering Progress Volume 43, page 160 (1947). Also Organic Syntheses Collective Volume 1 for alternate procedures. I worked out this procedure by myself in my lab, and it gives good results. That such a simple procedure, using such easily obtained materials, so effectively subverts the feds' control over tartaric acid shows what a bunch of ninnies they really are.

    To make tartaric acid suitable for use in making the tartaric salt of LSD, weigh out 10 grams of cream of tartar, and put it into a 100 ml beaker. I used McCormick brand, and it was nicely white and fluffy. Other brands will do, so long as they too are white and fluffy.

    To the 10 grams of cream of tartar, add water until the 50 ml mark is reached in the beaker. This produces a milky white suspension. Stir for a
    while to try to dissolve as much as possible, then add 10 ml 37% lab-grade hydrochloric acid. The mixture of calcium tartarate and potassium hydrogen tartarate that comprises cream of tartar reacts to form tartaric acid, along with KC1 and CaCl2- A clear solution results after about a minute of stirring.

    Now the water and excess hydrochloric acid are removed by vacuum
    evaporation. It is preferable to use a vacuum here, as heating at normal
    pressure may result in isomerization of the tartaric acid, and the replacement of some of the hydroxyl groupings in tartaric acid with chlorine. Also, hydrochloric acid was used here instead of sulfuric because the reaction is much faster, and the excess HC1 is removed during the evaporation. The solution should be evaporated down to a volume of about 10 ml. It will be yellowish in color, and have crystals of tartaric acid floating around in it, along with KC1 and CaCl2.

    Next, add 100 ml of 91% isopropyl alcohol, and dissolve the crystals of tartaric acid. KC1 and CaCh will not dissolve, and should be filtered out. 91% isopropyl alcohol is chosen because it is available at the drugstore, is not too good a solvent for tartaric acid for crystallization, and is less likely to form esters with tartaric acid than ethyl or methyl alcohol.

    The isopropyl alcohol is evaporated under a vacuum to 50 ml volume, and the first crop of white crystals of tartaric acid collected. This amounts to about 4 grams after drying. Further evaporation yields additional crops of crystals. Vacuum evaporation is used so that heating does not contribute to the formation of the ester isopropyl tartrate.
     
  14. ancient powers

    ancient powers Member

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    Lysergic Acid

    All of the production methods from here on out use lysergic acid as the starting material. These methods may be preferable if the alkaloids have been extracted from seeds rather than ergot, because the crystallization of lysergic acid affords an excellent opportunity to remove the clavine alkaloids present in the seeds.

    Two methods will be presented here. Method number one uses easily available KOH and methanol to cleave the amides to lysergic acid. Method number two uses hydrazine hydrate, which can be made from bleach and ammonia according to the directions in the previous chapter. The first method gives about 50% yield, while the yield in the second method is better. Both methods give a mixture of regular and iso lysergic acid, leading to mixtures of regular and iso-LSD. This makes the chromatographic separation procedure a must for all methods using the lysergic produced according to the directions given here.

    Method One

    Ten grams of lysergic amides extracted from the crops are dissolved in 200 ml of methanol containing 11 grams KOH. The methanol is then removed at once by distillation under a vacuum. To the residue in the flask, then add 200 ml of an 8% solution of KOH in water. This mixture should then be heated on a steam bath for one hour.

    Next, the reaction mixture should be cooled, and sulfuric acid added to it until it reaches pH 3. This results in the precipitation of crude lysergic acid having a dark color. The acid solution should next be extracted several times with ether. These extractions remove a lot of the lopped off portions of the
    lysergic amides, and lighten up the color of the lysergic acid. The acid suspension should next be filtered to yield dark colored crude crystals of
    lysergic acid.

    These crude crystals should be transferred to a beaker, and taken up in solution with two 200 ml portions of ethyl alcohol containing a few mis of strong ammonia. The residue which does not dissolve is inorganic, and can be discarded.

    The alcohol solution of lysergic acid should be evaporated to dryness under a vacuum. The crystals should be ground quickly while soaking for a short period of time in 50 ml methanol to remove colored impurities, then filtered. This yields about 2Y2 grams lysergic acid. It should be dried in a vacuum dessicator, then stored in the freezer. The lysergic acid even after vacuum-drying holds one molecule of water as part of the crystal structure. This is not a problem if the method given in Chapter 6 is used. Other synthesis
    methods require the removal of this water of crystallization, and it is tough.
    A vacuum of 2 mm Hg and a temperature of 140° C is needed to remove it.
    Such methods are best avoided if possible. Reference: Journal of Biological Chemistry, Volume 104, page 547.

    Method Two

    As mentioned before, this method gives higher yields, and so it is highly recommended. An increase in yield from 50% to 75% translates into 50% more LSD produced from the crops. This is well-worth the hassle involved with scrounging up or making some hydrazine hydrate.

    To do the hydrolysis, 15 grams of lysergic amides from the crops is put into a 500 ml flask along with a solution made up of 150 ml ethyl alcohol, 150 ml water, and 100 grams KOH. Next, 15 ml of hydrazine hydrate is added. This hydrazine should be the monohydrate, which is 64% hydrazine. If a weaker variety has been scrounged up, this can be made to work by adding more, and using less water.

    Now the flask should be fitted with a condenser, and flushed with nitrogen. Then heat the flask in an oil bath to gentle boiling for 4 hours. A slow stream of nitrogen to the flask during the reflux averts the danger from hydrazine.

    The flask is next cooled, and the contents poured into a sep funnel of at least 1000 ml capacity. The batch is then extracted with 600 ml ether, followed by 600 ml of an 85-15% mix of ether and alcohol. Finally, one more extraction with 600 ml of 85-15% ether-alcohol is done.

    All of the desired product should now be extracted into the solvent, and out of the water. This fact should be checked using a black light to look for the characteristic blue fluorescence. The combined solvent extracts should now be lowered to a pH of about 2 using HC1. At this point, a precipitate should form, and it should be filtered out. The precipitate should be washed free of
    entrained product with 4-1 ether-alcohol, and the washing added to the rest of the filtered solvent.

    Now 2750 ml of water should be added to the solvent, and the mixture placed in a gallon and a half glass jug or 5000 ml beaker. To this should be added 3 portions of cation exchange resin in H* cycle. Cation exchange resin is a common item of commerce used in deionized water systems. Check the yellow pages under "water" and see which of the local Culligan men offer deionized water systems.

    The deionizers come in two-tank systems with one tank packed with cation exchange resin to remove calcium, magnesium and sodium from the water. The other tank has an anion exchange resin to remove chlorides, sulfates, and so on. It is no great task to buy cation exchange resin from these outlets. The resin consists of tiny plastic beads coated with the exchanger. In the case of the cation exchangers, this is generally a sulfonate. "In H* cycle" means that the resin is charged up and ready to go. This is generally done by soaking the resin in 20% sulfuric acid in water for a while, then rinsing with distilled water. Check the directions on the container of resin. Steer clear of mixed resins that contain both anion and cation exchangers. If the Culligan man is too stupid to know the difference, or doesn't know what he has, keep looking until you find one who knows his business.

    The treatment with three portions of cation exchange resin in H* cycle should be done as follows: Each portion of resin should weigh about 15 grams. The first portion is added, and then the mixture should be stirred strongly or shaken for about 10 minutes. The product will come out of the liquid, and stick to the resin. The resin should be filtered out, and kept in the fridge while similar treatment proceeds with the next two portions of cation exchange resin.

    All of the product should now be out of the liquid and on the resin. This should again be checked using the blacklight. The resin portions are now combined, and soaked in 300 ml of 10% NRjOH in water for 30 minutes with stirring. This brings the product off the resin, and into the ammonia solution. The slurry should now be filtered to give a brown liquid which is kept in the
    fridge. The resin should be treated again with 300 ml of 10% NHtOH, and filtered.

    Now the 600 ml of ammonia solution containing lysergic acid should be evaporated down in a vacuum to a volume of 50 ml, and this remaining liquid kept in the fridge overnight at 4 C to yield a precipitate of about 5'/z grams of 96% pure lysergic acid. It consists of lysergic acid and iso-lysergic acid in about a two-to-one ratio.

    The resin can be used over and over again by recharging in 20% sulfuric acid solution, and rinsing with distilled water. Reference: Chem Abstracts, Volume 69, column 36323 (1968) Czech patent 123,689


    Notes :

    1. The blacklight is your friend, and is very useful in spotting the
    product, but don't overuse it as UV is quite harmful to the
    product. The blacklight should be a fluorescent tube, and not
    some black painted light bulb.

    2. All work described in this chapter should be done under red or
    yellow darkroom lighting.
     
  15. ancient powers

    ancient powers Member

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    Hydrazine Sulfate Synthesis Optimized OTC Procedure

    The hydrazine sulfate synthesis which I have done successfully many times is a slightly modified procedure based on the method described by GB392845. Everything is OTC ingredient optimized and the yields are high, the hydrazine is freebased into methanol by a modified procedure similar to GB876038. This results in hydrazine hydrate in methanol. However, if the methanol contains sufficient sodium methoxide or potassium methoxide, by methods such as US2278550 or US4267396, then anhydrous hydrazine in methanol is the result :). Good yields of alkali azides may be obtained by reaction of the methanolic hydrazine with isopropyl nitrite. See US1628380, US5098597, US5208002. Small scale syntheses for alkali azides are favored by anhydrous methods in my experience.

    There is no problem using OTC materials if you compensate the approach and adjust for total water, and keep to the molar proportions. I could write up the details for Hydrazine Sulfate OTC optimized quick and easy. The reaction is a bit complicated by foaming at a point, so a lot of empty space in the reaction vessel is required, as headroom for preventing overflows. This constraint places the yield limit to about 140 grams of hydrazine sulfate for a "pickle jar" sized reaction vessel. Actually I do the reaction in a 4 liter erlenmeyer equipped with a 4 liter foam overflow return reservoir. A 6 liter flat bottomed florence flask would be better. The oxidation of urea proceeds just fine in the cold and I prechill the basified hypochlorite to 10 below 0 degrees centigrade. Get it stirring with a large stirbar, and pour the warm urea/gelatine solution into the vortex of the mixture. I let the reaction proceed on its own gentle exotherm for about 1 and one half hours, and through to a point of 75 per cent subsiding of foaming, before applying any supplemental heating to finish the oxidation. The foaming can get wild when the heat is applied if the reaction has not proceeded far enough towards completion before the heating is applied. This synthesis goes through some interesting color changes which help to track the progress of the reaction towards completion.

    About two minutes after pouring in the warm urea/gelatine solution the mixture changes from light yellowish green to white and the mixture foams to double its volume. After ten minutes the stiff foam begins to break free under the influence of the stirbar and slowly subsides while becoming more mobile and stirrable. After one hour the foam has subsided to about two thirds its initial highpoint. A slight orange color is noted. The foam continues to fall and then heat is applied very gradually, because just a small heating will kick the reaction back into a vigorous foaming, and this is when the overflow may occur. The idea is to just nudge the reaction rate a bit, and then let it proceed to run on its own energy again. The orange color will become very pronounced and darker at this stage of the reaction, as the foaming subsides nearly completely. At this point it is safe to increase the temperature rapidly up about 85 or 90 degrees centigrade to drive the reaction to completion. At the endpoint of the reaction the dark orange color will dissipate almost completely, and the solution color will suddenly fade to a very pale slight yellow tint, almost clear. When you see that color change, the reaction is complete. Peak the temperature, and then discontinue heating. Immediately remove the flask to a cool water bath.

    Experimental:

    1500 ml of 10 per cent sodium hypochlorite is placed into a 2 liter glass jar, lightly sealed with a lid, and placed into the freezer overnight to chill to 15 below 0 degrees centigrade. Into the prechilled 1500 ml of "liquid pool chlorinator" is dropped a stirbar and while stirring, 194 grams of fine prilled NaOH is added into the vortex at a rate as fast as it will dissolve and not accumulate on the bottom. Because of the exotherm, the addition must be done in two portions in order to prevent excessive warming and thermal decomposition of the hypochlorite. The first portion of the NaOH should be about 110 grams, and then the solution should be rechilled in the freezer to about 0 degrees centigrade before adding in the same manner the remaining 84 grams of NaOH. The basified hypochlorite is then returned to the freezer for keeping, and to rechill to 15 below 0 degrees centigrade for its use later in the hydrazine synthesis.
    In a separate half liter jar having a lid, 132 grams of urea is dissolved in 70 ml of hot distilled water.

    In yet another half liter jar having a lid, 1.8 (one and eight tenths gram) grams of gelatine is dissolved in 70 ml of hot distilled water.
    Shaking of these containers will facilitate the solution, and supplemental warming of the containers in a hot water bath will also be required. After these warm solutions are prepared, and all solids are dissolved, the two solutions are combined just before use, and the combined solutions are kept standing in a bowl of warm water to mainatain everything in solution and prevent the mixture from congealing, which will occur if the mixture is allowed to cool.

    A 4 liter Erlenmeyer flask is placed upon a stirrer hotplate and a three inch stirbar is placed in the flask. The heat remains off. Into the neck of the flask is placed a wide mouth plastic funnel of one gallon capacity, the neck of the funnel is enlarged with a bushing cut from a two inch length of one and five eighths OD, one and one quarter ID, tygon vinyl tubing, for a snug fit in the neck of the flask. The plastic funnel serves as an overflow reservoir and return path for any foaming which may exceed the capacity of the flask during the reaction.

    The previously prepared, cold basified hypochlorite solution is poured into the flask and the stirrer started without any heating. The previously prepared, warm combined solution of urea and gelatine is poured through the funnel into the well stirred hypochlorite.

    After a couple of minutes the reaction will initiate, and after fifteen minutes the foaming mixture will occupy twice the original volume, and the foam will temporarily be very rigid and motionless, but this will not persist for more than a few minutes. The foam will begin to very slowly disintegrate and stir down. The foam is viscous enough to cause uncoupling of the stirbar on the stirplate, at speed settings above 40 per cent, so it is better to have it stir successfully at a conservative setting.
    About one hour after the reaction is begun, supplemental heat is applied, cautiously at first, because about ten minutes later a renewed episode of foaming will occur. This is a very transient and less viscous foaming which dissipates quickly. The onset of this foaming will be indicated by a dark orange color about the reaction mixture. When this episode of foaming occurs the reaction is nearing completion, and with increasing heating of the mixture to about 90 degrees centigrade, the reaction is complete at about one and one half hours from the beginning.

    I do not even measure the temperature endpoint, but establish the endpoint by observing the color shift from orange to a very pale yellow, almost clear......very light tint to the solution. When the mixture has become hot enough, and all the foaming has subsided, the moisture will begin to reflux on the walls of the flask above the liquid and in the neck area of the flask. This happens when a mixture is nearing the boiling point, which is plenty hot enough for this reaction. So when the refluxing moisture and color change have occured, the heating is stopped and the flask is removed to a cooling bath. After the mixture has cooled down, it is acidified by the dropwise addition of dilute sulfuric acid, with stirring, and using the same overflow funnel setup as before. 1100 ml of density 1.260 new battery electrolyte, which is 35 per cent sulfuric acid, is added at a rate of 3 or 4 drips per second to the stirred solution, and an exotherm is evident during the neutralization / acidification. The acidified mixture is cooled to about 10 to 15 degrees centigrade for precipitation of the hydrazine sulfate, and allowed to stand for several hours to complete the precipitation. Do not chill the mixture very cold or huge amounts of Glaubers Salt (hydrated sodium sulfate) will settle out along with the hydrazine sulfate.

    The hydrazine sulfate is filtered and dried, yield is 159 grams.
    In the previous communication about the usefulness of urea, I failed to mention a patent which shows the usefulness of urea in synthesis of methylamine. EP 0037862 discloses a high yield synthesis for methylamine nitrate. Also see GB1548827 for a closely related synthesis. It is my guess that paraformaldehyde would react with a diluted urea/ammonium nitrate eutectic. There was a mention of the nitrate process at the Hive, but no details or followup information was posted in the methylamine FAQ. Also see GB168333.
     
  16. ancient powers

    ancient powers Member

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    Ok guys im getting way better at this. I made a MGS tincture a few months back. 100gs of seeds were used and I was able to reduce the LSA content to 1mg LSA + sediment per 2ml of tincture. With personal testing I consumed 6ml which was very strong and equal to any 3mg LSA experience I commonly take.

    There was still a little residue of peppermint oil which I had washed out when recleaning and reducing the sediment volume. The effects were most impressive. Naseaua and vomitting were nada. Flavor wasnt too bad except peppermint oil residue. I feel if having not used peppermint oil the tincture would be flavorless in water or juice. BTW LSH conversion with peppermint oil is urban legend from my experience.

    On further meditation into perfecting my art here I will share with the world an absolute miracle for those who would love to harness this plant ally.

    For a 1oz (30ml) tincture of MGS or HBWRS you will need 100gs MGS or 10g HBWRS. Clean off fuzz with fingernails if using HBWRS. Blend seeds in a blender with a double amount of vodka for a few minutes and pour into a clean jar. Put jar into freezer for 15min then shake. Let sit for 15min more in freezer and carefully pour off liquid into a bowl or container, leaving the sediment at the bottom.

    Add another double volume of vodka to seed pulp/sediment, shake and repeat extraction. combine both liquid extracts and let sit overnite. Carefully pour off liquid leaving any sediment behind. Pour liquid into a ziplock freezer baggie and hang by top corner overnite.

    In the morning slide a paper clip above the sediment layer on the baggie. Make sure sediment layer is completely cut off from the above liquid layer with the paper clip. Move the baggie to point the other bottom corner down. Cut another small hole and gather liquid on a large glass baking dish. Evaporate dish with fan until dry. Scrape with clean razor blade and reconstitute in 1oz amber tincture bottle to 25ml vodka. This will yield 1mg LSA per 1ml plus all the companion alkaloids that set the LSA off.

    Very cool and mellow, Religious feelings, Quieted thoughts, Direct experience with the world around you and spiritual visions. Alters perception and the thought process in a very natural way!

    The evaporated extract can be dissolved in a ph8.5 ammonia/distilled water solution and extracted 4x with a small layer of naphtha or toulene. The solvant is evaporated for LSA freebase which can be stored in the freezer immediately or you dissolve 1 part tartaric acid to 3 parts LSA freebase in a small amount of vodka and evaporate in a cool dark place with fan or vacuum for LSA tartrate.
     
  17. ancient powers

    ancient powers Member

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    When larger quantities of seeds of Rivea corymbosa and Ipomoea violacea were available, the indole compounds could be obtained in preparative quantities. It was found that they were alkaloidal in nature and that they could be isolated by the usual methods used for the extraction and purification of alkaloids. For this purpose, the finely ground seeds were made alkaline with sodium bicarbonate, then extracted with ethyl acetate.

    The alkaloids were then removed from the extracts, which had been concentrated to a small volume in vacuum, with aqueous tartaric acid from which they were again shaken with ethyl acetate after making the mixture alkaline with a sodium bicarbonate solution.

    From the alkaloidial fractions thus obtained, the individual components visible in the thin layer chromatogram could be seperated by fractional crystallization, chromatography on aluminum oxide and silca gel layers, on a preparative scale. The seperated compunds were obtained in crystalline form and could be identified chemically.
     
  18. ancient powers

    ancient powers Member

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    :sunny:To release the alkaloids out of the plant. It must first be dried or powdered. Cardboard, plywood or cookie sheets with a fan at room temp or outdoors works.

    Blenders cover the initial grinding then finish up using coffee grinders for a fine grind. If powdering rootbark or woody vines, you will want to macerate first by pounding down from the top of a length with a hammer. Then add to the blender then grinder.

    A acidic water solution would consist of a 5% solution of citric acid or vitamin c powder. This is made by measuring 5gs of citric acid or vitamin c to 100gs distilled water. Or until you have a ph4 solution.

    50g = 1ft dried san pedro skins which = 1 dose. 100gs if using pachanoi var.

    Simmer powder in minimal acidic/H2o solution for 20min. Strain and repeat cooking powder in fresh acidic/H2o solution 2x.

    Hang up solution in a clear ziplock baggie by a corner and allow all the sediment to settle to the bottom corner. Cut a small hole and gently remove sediment. Once all sediment is removed gather the solution on a large glass baking dish and evaporate in the oven at the lowest possible setting. 150F max.

    Once you have a wet solid dry with a fan at room temp.

    Scrape the dried residue with a fresh razor blade.

    You can either take this dry concentrated extract as is. I recommend vegetable juice as a mixer and water as a shooter.

    Experimental would be to take the powder and mix powder in a beaker or open mouth jar or glass with acetone, naphtha or MEK. You will want to use a generous amount at first to reduce the amount of times you will have to decant the solvant.

    This should remove most solvant soluble plant material. MEK will also remove the non mescaline alkaloids ref 69ron.

    Simply mix the solvant and stir and allow to set for many hours with swirling. Allow to alkaliods to settle and carefully decant solvant, which means to pour off solution. Do not worry about pouring all solvant off after further cleaning we can evaporate the remaing amounts.

    After the first pour depending on the clarity of the solvant add a little more swirl and decant again. Then pour on evap dish and dry with fan. You will want to add a little fresh solvant to the container to swirl and wash any possible alkaliodial residue from it and add to the evap dish.
     
  19. ancient powers

    ancient powers Member

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    On the 16th of April 1943, upon recrystallizing d-lysergic acid diethylamine tartrate, which I had produced from natural lysergic acid and diethylamine by way of the lysergic acid hydrazide and azide, I suddenly baecame strangely inebriated. The external world became changed as in a dream. Objects appeared to gain in relief; they assumed unusual dimensions; and colors became more glowing. Even self-perception and the sense of time were changed. When the eyes were closed, colored pictures flashed past in a quickly changing kaleidoscope. After a few hours, the not unpleasant inebriation, which had been experienced whilst I was fully concious, disappeared.

    What caused this condition? Subsequent systematic self-experimentation with the chemicals that I had used that day were to provide the answer. Lysergic acid diethylamide was tested, amongst other substances, as it was possible that a drop had fallen on my fingers and had been absorbed by the skin. I commenced my experiments on this compound by taking 0.5ml of a 0.5 per mille aqueous solution, corresponding to 0.25 mg of d-lysergic acid diethylamide tartrate. This extremely small quantity proved to be a substantial overdose.

    A state of inebriation followed, lasting for a number of hours and filled with dramatic experiences, which have been described in former publications. This is how the most active psychotomimetic, hallucinogenic compound which subsequently attained great importance under the name of LSD 25 (Delysid) in experimental psychiatry and, recently, in psychotherapy as well.
     
  20. ancient powers

    ancient powers Member

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    Mescaline Extraction Technique

    I have searched far and wide online for practical realistic mescaline extraction. I have tried a thousand different approaches to consuming the cactus ally. This is the perfected art of my craft. I just wanted it to be easy for someone like minded to find the truth. Enjoy. e

    Using 2.5ft of fresh pachanoi skins (1250g of fresh cactus weight). Or 125g of dried cactus. Skin the outer layer of cactus by cutting cactus column into 3 inch chunks. Cut down between the white and dark green inner layer.

    Blend skins in a blender by adding them through the small opening in the lid 1 by 1. Liquify into a cactus smoothie and pour into a pot on med heat. Bring cactus smoothie to a boil while stirring. Bring to a simmer and stir until you have a dark green thick cactus juice. Fill a large 80oz pickle jar halfway with cactus juice (40oz, 5 cups, 1250ml). Or 125g of dried cactus skins (powdered) to 8 cups of distilled water Add 1 tbsp of NaOH (sodium hydroxide) per 150ml of cactus juice to the jar of juice (1250 divided by 150 = 8.33 or 8tbsp). Cap and roll Jar 100x. crack open the lid and allow juice to basify for 30 min. Roll jar Before adding the xylene to mix up the basified alkaloids . Add 1/3 the amount of xylene to cactus juice. Roll jar 100x and allow layers to separate (about an hour). Remove upper xylene layer with a small clear cup (a clear cap from your liquid laundry detergent works nice).

    Do not remove all the xylene from the juice jar. Leave a small layer to avoid contaminating the xylene extract with cactus fat. Add xylene extract to a clean jar. Add 2 oz of acidic water (1/2 tsp citric acid per 6oz distilled water) to volume of xylene extract. Shake jar for 5 min. Allow layers to separate then carefully pour off upper xylene layer back into cactus juice jar. Leave a small layer of xylene with your acidic water so you don’t lose any alkaloids. Extract cactus juice and xylene extract 3x. Gather all the acidic water with small layer of xylene together into a clean jar. Freeze solution until bottom layer is frozen solid. Pour off remaining xylene and scrape residual cactus fat off with a spoon.

    Wipe down inside of jar with a paper towel then rinse with cold water. Allow frozen solution to melt then pour onto evaporation dish. Allow solution to fully evaporate into a gooey amber resin. Scrape with razor blade. Break up residue over a period of days until dry enough to crush in into powder. Mescaline is 00.12% the fresh cactus alkaloid weight. 500mg of mescaline is the equivalent of 1 full blown psychedelic experience.(http://www.flashback.se/archive/tibetan.html#33 refer to the drugs and dosage section in 3.3).

    The cactus weight of fresh skins per 40oz of juice or 2.5ft of pachanoi skins = 1250g. 1250 x .0012 = 1.5g or 1500mg mescaline weight

    (http://www.biopark.org/peru/mescaline-healing.html refer to paragraph 20). If 2.5ft of pachanoi weight = 1250g fresh weight. Then it should dry to approximately 125g dried skins. so 1 foot cactus column worth of skins should weight 500g fresh or 50g dried. 500 x .0012 = 0.6g or 600mg of mescaline per 1 foot cuttings.

    The total alkaloid weight of your procured product should weight about 3 grams. Split it 3 ways and you have 3 x 500mg mescaline trips.

    Happy Tripping!
     

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