Geodesic Chemistry.

All I can say is the fact that there is no information on this chemical and its novelty could be the very thing the universe needs to solve the equation of life. I will at least try to answer this one question in my life, does this "imaginary" chemical really matter at all? If so why have we heard nothing? Why, despite its substructure being stable in other compounds, has it not been documented and synthesized. As the man at the research institute Dennis McKenna established, the amide off an aromatic ring will be too high ph to be active, (why not try a salt?). All is still speculation on a simple shape still. I got another reply from a company that said they flat out would not make me the chemical as it is a "hallucinogen" and is related to the LSD molecule, and thus is "illegal?"

Should someone make a chemical entirely unknown "illegal" before its ever been made and tested?

 

Lets kick some ass azygous, I think I've finally caught up with your thinking. PM me we need to talk

 

Mono Atomic Gold Particles may be a better catalyst for the LSA to LSD converter.

 

Wow, the possibilities are endless. I'm gonna get a magic marker, draw a meth molecule on a volleyball, and get tweaked out my mind. Meanwhile, back in the real world....

 

lol this is fail simply wont work, I hate to be the bearer of bad news but this simply wont work... If you want me to get into more depth i will but i choose not to due to the fact your brain can't handle it nor can mine right now...

 

so is all this bullshit to convert LSA to LSD? if so, this is dumb.. I enjoy LSA entirely and find it sort of redundant to desire to convert it, in it's righteous own existence into the other, lsd. If you know this much about the chemicals themselves, creating LSD should be a peice of cake for you. enjoy the cake, but leave the lsa alone man..

 

man i had to respond again, what mind would complex the thought of aiding such a conversion with monoatomic golds.. someone has been listening to lawrence gardener or someone way to closely.. seask is right.. other than that, what a lame thread do anyone know what the fuck they are talking about? Morning glory is the best for LSA for my belly, anyhow.. I mean, I study chemistry aimed from Ferenc Fulop, he studied LSA and any optical activity.. but this thread is mumbo jumbo, good luck and cheers for day dreaming

 

nvm

 

dat skeet is wack!

 

I learned a lot after reading your posts guys. Things like this help me feel that I am not alone and other people are doing what I've been doing for quite some time now.

 

Trippy thread. Great thought/imagination experiment.

Peace & Love,
Spicey Cat
Purrr!

 

This thread will never die! I still dont know if it would really work. Gettin the amount of LSA needed is the hardest part.

 

... if the reaction occupied a sufficiently small space, it could work.

 

Ok if you eventually come to realize how to make LSD from LSA?

 

Hey finally got back into my account Yeah follow the research at www.geodesicchemistry.com the work I do there is study all the chemicals in TIKAL and PIKAL using a program called Millsian. I am using this program to build a framework of the 5-HT receptor as well as aspects of the Sigma one receptor systems. This will help prove if T-LSD or 4-DBT whatever it be named will work as well as how they and many other molecules work on these receptors. These frameworks may also give insight into the LSA to LSD conversion in a way much similar to how these patterns gave rise to an understanding of new patterns and new molecules. Not much documentation is present on my website quite yet but coming shorty but it has about %85 of the data collected on the server I need to prove/disprove theories as well as make some new profound discoveries. Hope this thread has sparked imagination no computer models on the process have been made by me at this point. Using the right theory of physics you might be able to nail down the precise dimensions to focus the energy in just the right way.===== Anyhow Peace best of luck to anyone still testing these waters. I have moved on to the next step my research has led me to thanks for all the comments and bill you helped talk me through some stuff so if you are interest or anyone about the process of my site let me know

 

then you have a readily available source of the chemicals needed to make LSD from Morning Glories or HBWR seeds.

 

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.

 

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.

 

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.

 

good post ancient powers always like readying LSD chemistry.. so he actually dosed himself doing the "lysergic acid hydrazide" approach? So Albert Hofmann knew all along that a swift transition between LSA to LSD was feasible even chemically.