LSD-25 Synthesis

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LSD-25 Synthesis




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LSD-25 Synthesis from "Psychedelic Guide to the Preparation of the Eucharist"

Preparatory arrangements

Starting material may be any lysergic acid derivative, from ergot on rye grain or from culture, or morning glory seeds or from synthetic sources. Preparation #1 uses any amide, or lysergic acid as starting material. Preparations #2 and #3 must start with lysergic acid only, prepared from the amides as follows:

10 g of any lysergic acid amide from various natural sources dissolved in 200 ml of methanolic KOH solution and the methanol removed immediately in vacuo. The residue is treated with 200 ml of an 8% aqueous solution of KOH and the mixture heated on a steam bath for one hour. A stream of nitrogen gas is passed through the flask during heating and the evolved NH3 gas may be titrated is HCl to follow the reaction. The alkaline solution is made neutral to congo red with tartaric acid, filtered, cleaned by extraction with ether, the aqueous solution filtered and evaporated. Digest with MeOH to remove some of the coloured material from the crystals of lysergic acid.
Arrange the lighting in the lab similarly to that of a dark room. Use photographic red and yellow safety lights, as lysergic acid derivatives are decomposed when light is present. Rubber gloves must be worn due to the highly poisonous nature of ergot alkaloids. A hair drier, or, better, a flash evaporator, is necessary to speed up steps where evaporation is necessary.

Preparation #1


Step I. Use Yellow light


Place one volume of powdered ergot alkaloid material in a tiny roundbottom flask and add two volumes of anhydrous hydrazine. An alternate procedure uses a sealed tube in which the reagents are heated at 112 C. The mixture is refluxed (or heated) for 30 minutes. Add 1.5 volumes of H2O and boil 15 minutes. On cooling in the refrigerator, isolysergic acid hydrazide is crystallised.

Step II. Use Red light


Chill all reagents and have ice handy. Dissolve 2.82 g hydrazine rapidly in 100 ml 0.1 N ice-cold HCl using an ice bath to keep the reaction vessel at 0 C. 100 ml ice-cold 0.1 N NaNO2 is added and after 2 to 3 minutes vigorous stirring, 130 ml more HCl is added dropwise with vigorous stirring again in an ice bath. After 5 minutes, neutralise the solution with NaHCO3 saturated sol. and extract with ether. Remove the aqueous solution and try to dissolve the gummy substance in ether. Adjust the ether solution by adding 3 g diethylamine per 300 ml ether extract. Allow to stand in the dark, gradually warming up to 20 C over a period of 24 hours. Evaporate in vacuum and treat as indicated in the purification section for conversion of iso-lysergic amides to lysergic acid amides.


Preparation #2


Step I. Use Yellow light


5.36 g of d-lysergic acid are suspended in 125 ml of acetonitrile and the suspension cooled to about -20 C in a bath of acetone cooled with dry ice. To the suspension is added a cold (-20 C) solution of 8.82 g of trifluoroacetic anhydride in 75 ml of acetonitrile. The mixture is allowed to stand at -20 C for about 1.5 hours during which the suspended material dissolves, and the d-lysergic acid is converted to the mixed anhydride of lysergic and trifluoroacetic acids. The mixed anhydride can be separated in the form of an oil by evaporating the solvent in vacuo at a temperature below 0 C, but this is not necessary. Everything must be kept anhydrous.

Step II. Use Yellow light


The solution of mixed anhydrides in acetonitrile from Step I is added to 150 ml of a second solution of acetonitrile containing 7.6 g of diethylamine. The mixture is held in the dark at room temperature for about 2 hours. The acetonitrile is evaporated in vacuo, leaving a residue of LSD-25 plus other impurities. The residue is dissolved in 150 ml of chloroform and 20 ml of ice water. The chloroform layer is removed and the aqueous layer is extracted with several portions of chloroform. The chloroform portions are combined and in turn washed with four 50 ml portions of ice-cold water. The chloroform solution is then dried over anhydrous Na2SO4 and evaporated in vacuo.


Preparation #3


This procedure gives good yield and is very fast with little iso-lysergic acid being formed (its effect are mildly unpleasant). However, the stoichometry must be exact or yields will drop.

Step I. Use White light


Sulfur trioxide is produced in anhydrous state by carefully decomposing anhydrous ferric sulfate at approximately 480 C. Store under anhydrous conditions.

Step II. Use White light


A carefully dried 22 litre RB flask fitted with an ice bath, condenser, dropping funnel and mechanical stirrer is charged with 10 to 11 litres of dimethylformamide (freshly distilled under reduced pressure). The condenser and dropping funnel are both protected against atmospheric moisture. 2 lb of sulfur trioxide (Sulfan B) are introduced dropwise, very cautiously stirring, during 4 to 5 hours. The temperature is kept at 0-5 C throughout the addition. After the addition is complete, the mixture is stirred for 1-2 hours until some separated, crystalline sulfur trioxide-dimethylformamide complex has dissolved. The reagent is transferred to an air- tight automatic pipette for convenient dispensing, and kept in the cold. Although the reagent, which is colourless, may change from yellow to red, its efficiency remains unimpaired for three to four months in cold storage. An aliquot is dissolved in water and titrated with standard NaOH to a phenolphthalein end point.

Step III. Use Red light


A solution of 7.15 g of d-lysergic acid mono hydrate (25 mmol) and 1.06 g of lithium hydroxide hydrate (25 mmol) in 200 ml of MeOH is prepared. The solvent is distilled on the steam bath under reduced pressure. the residue of glass-like lithium lysergate is dissolved in 400 ml of anhydrous dimethyl formamide. From this solution about 200 ml of the dimethyl formamide is distilled off at 15 ml pressure through a 12 inch helices packed column. the resulting anhydrous solution of lithium lysergate left behind is cooled to 0 C and, with stirring, treated rapidly with 500 ml of SO3-DMF solution (1.00 molar). The mixture is stirred in the cold for 10 minutes and then 9.14 g (125.0 mmol) of diethylamine is added. The stirring and cooling are continued for 10 minutes longer, when 400 ml of water is added to decompose the reaction complex. After mixing thoroughly, 200 ml of saturated aqueous saline solution is added. The amide product is isolated by repeated extraction with 500 ml portions of ethylene dichloride. the combined extract is dried and then concentrated to a syrup under reduced pressure. Do not heat up the syrup during concentration. the LSD may crystallise out, but the crystals and the mother liquor may be chromatographed according to the instructions on purification.


Purification of LSD-25


The material obtained by any of these three preparations may contain both lysergic acid and iso-lysergic acid amides. Preparation #1 contains mostly iso-lysergic diethylamide and must be converted prior to separation. For this material, go to Step II first.

Step I

Use darkroom and follow with a long wave UV The material is dissolved in a 3:1 mixture of benzene and chloroform. Pack the chromatography column with a slurry of basic alumina in benzene so that a 1 inch column is six inches long. Drain the solvent to the top of the alumina column and carefully add an aliquot of the LSD-solvent solution containing 50 ml of solvent and 1 g LSD. Run this through the column, following the fastest moving fluorescent band. After it has been collected, strip the remaining material from the column by washing with MeOH. Use the UV light sparingly to prevent excessive damage to the compounds. Evaporate the second fraction in vacuo and set aside for Step II. The fraction containing the pure LSD is concentrated in vacuo and the syrup will crystallise slowly. This material may be converted to the tartrate by tartaric acid and the LSD tartrate conveniently crystallised. MP 190-196 C.

Step II. Use Red light


Dissolve the residue derived from the methanol stripping of the column in a minimum amount of alcohol. Add twice that volume of 4 N alcoholic KOH solution and allow the mixture to stand at room temperature for several hours. Neutralise with dilute HCl, make slightly basic with NH4OH and extract with chloroform or ethylene dichloride as in preparations #1 or #2. Evaporate in vacuo and chromatograph as in the previous step.

Lysergic acid compounds are unstable to heat, light and oxygen. In any form it helps to add ascorbic acid as an anti- oxidant, keeping the container tightly closed, light-tight with aluminum foil, and in a refrigerator.

Synthesis of d-LSD maleate or tartrate from lysergic acid with POCl3


Ref:
Johnson, Ary, Teiger, Kassel. "Emetic Activity of Reduced Lysergamides." Journal of Medicinal Chemistry. 16(5):532-537. 1973.
Related:
Huang, Marona-Lewicka, Pfaff, Nichols. "Drug Discrimination and Receptor Binding Studies of N-Isopropyl Lysergamide Derivates." Pharmacology, Biochmistry and Behavior. 47(3):667-673, 1994.
Oberlender, Pfaff, Johnson, Huang, Nichols. "Stereoselective LSD-like Activity in d-Lysergic Acid Amides of (R)- and (S)-2-Aminobutane." Journal of Medicinal Chemistry. 35(2):203-211, 1992.
Hoffman-AJ, Nichols. "Synthesis and LSD-like Descriminative Stimulus Properties in a Series of N(6)-alkyl Norlysergic Acid N,N-Diethylamide Derivates." Journal of Medicinal Chemistry. 28:1252-1255, 1985.
NOTE: JMC 35(2):203-211 has some amazing stereoviews of LSD which might interest non-chemists who like to cross their eyes.
Under reduced light (or red light) a stirred solution of 3.15g (11 mmol) of d-lysergic acid monohydrate and 4.45g (99 mmol) of diethylamine was brought to reflux by heating. Heat was removed, and reflux was maintained by the addition of 2ml (3.4g, 22mmol) of phosphorous oxychloride (POCl3) over a 2 minute period. The mixture was then refluxed for an additional 4-5 mins until an amber-colored solution resulted. The solution was brought to room temperature and was washed with 200ml of 1M NH4OH. The CHCl3 solution was dried (MgSO4), filtered, and concentrated under vacuum (not allowing the solution to exceed 40 degrees C). The last traces of the solvent were removed at 2-5 mm. The viscious residue was dissolved in a minimum amount of MeOH and acidified with a freshly prepared 20% solution of maleic acid in MeOH. Crystallization occured spontaneously. The needles were filtered, washed with cold MeOH and air-dried. Yield was 66% after further purification by column chromatography over alumina (Brockman) and elution with 3:1 benzene-chloroform. The chromatography takes appx 8-9 hours. Alternatively, it can be crystallized as the (+)-tartrate from MeOH. After crystallizing from cold MeOH, it is diluted with ethyl acetate, filtered and the the crystals are washed with ethyl acetate.
This procedure also works for primary amines and small dialkyl amines. LSD, however, probably remains the most worthwhile product. Other interesting amines might be the N-ethyl-N-propyl derivative (LEP) and the morpholide (LSM-775). 75ug of the morpholide have been reported to have been as effective as 50ug of d-LSD but with 45 min onset (vs 1 hour) and a 1 hour peak (vs 4 hours). The procedure would probably work well for LEP, but yields would be reduced for the morpholide. Other N(20)-alkyl-lysergic acid derivatives tend to be more than 10 times less potent than LSD if not effectively inactive. N(6)-ethyl- (and -allyl- and -propyl-) derivates of LSD may be more active than LSD itself, but synthetic routes to these chemicals presently start with LSD and yields would probably inhibit their appearance on the illicit market. (N(6) is the other nitrogen on the ring structure in addition to the N(1) pyrrole/indole nitrogen). Derivatives of LSD (besides LSA/LA-111 and lysergic acid) are not scheduled, but would be prosecutable under the designer drugs act after testimony from a DEA agent that _in their opinion_ the defendant was planning to distribute them.
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Now the only reason I wanted to post this obviously copied recipe is because I feel I have broken the first code of the LSA extraction for the basis of making LSD. After many experiments using the acid / base method for extractions. If its is an alkaloid then the acid / base tek will work for whatever alkaloid it is. LSA happens to be an alkaloid. If you look at the first part KOH is used. KOH is comparable to NaOH. You could probably use NaOH in place of KOH and still have success.

 

according to the directions, a source of lysergic acid amide (LSA) is dissolved into 200ml of methanol with some KOH in it. Methanol can be purchased as HEET in your local store. If you read the ingriedients it says bottle contains methanol. It probably doesnt matter how much KOH as long as it becomes a basic or ph 8+. I would assume 1 tbsp of KOH or NaOH in 200ml methanol would be sufficient. It says that the methanol is removed through a vacuum but you could allow to evaporate and Im sure it would be fine. The residue which I assume will be oily is treated in a 8% aqueous solution of KOH. A ml is = to 1g so 8% of 200ml is 16g. So a solution of 16g KOH is dissolved into 200ml distilled water and added to the flask or jar. The flask or jar is heated in a steam bath for 1 hr while a stream of nitrogen gas is passed through the flask. This would be done with a rubber stopper with two holes one hole feeds nitrogen gas gently into the basic aqueous soution while the other hole vents what appears to be converted into ammonia gas. I believe there is a misprint in that the writer asks if HCL is to be used following. I believe the nitrogen converts the LSA in just plain LS. Lysergic acid not lyseric acid amide.

 

The solution is then made neutral which is 7 out of 14. 0-6 = acidic. 7 = neutral. 8-14 = alkaline. You use tartaric acid which is found in wine. You could probably evaporate wine and extract tartaric acid. but im sure its available for sale. this is added to make the solution neutral by bringing the ph down from being so high on the KOH. The soution is then filtered through filter paper or coffee filter. The LS binds to the tartaric acid ceating LS tatrate during the salting phase after the nitrogen stream. So when you filter it, the solid LS tartrate crystals are caught on the filter. dissolved in ether, filtered and the filtered ether evaporated. then wash the crystals in methanol to clean them up. This should yield perfect LS tartrate crystals. At least you have a pure alkaloid in which to convert. When I can grasp the conversion portion and make it more easily understood. I will post.

 

The other possible option is common clandenstine practices of a/b extractions. You could use either KOH or NaOH as your basifying agents. Powder your woodrose, morning glories, stipa robusta, or ergot in a coffee grinder. Then dissolve in a solution of 1tbsp of basifying agent per 150ml of distilled water. I would think and it needs testing that xylene might be used since petrolium ether (naptha) is used to wash the seeds in original seed extraction teks. But either one is used to pull the basified alkaloid from the basified aqueous solution. The xylene is added to make 1 part xylene 2 part basic LSA water solution. The soluton is shaken for 5 mins and allowed to seperate. The xylene is removed by either freezing the solution till the water is frozen and the xylene can be poured off or by gathering it with a siphon hose, turkey baster or small cup. Water with a small amount of tartaric acid is then added to the extracted xylene and used to turn the basified LSA into LSA tartrate. shake for 5 min and extract the xylene layer. The xylene is then returned to the basified LSA water and the process is executed 3x. All three LSA tartrate waters are added together and evaporated. I believe you could use rubbing alcohol instead of distilled water in the salting process for quicker evaporation.

 

The seeds must be washed in petroleum ether (naptha) to extract the negative plant material from the seed powder. The seed powder can then be dissolved in basified water (1tbsp per 150ml). Then I would use naptha to extract the LSA. I believe it would be soluble in naptha in a basic state like DMT is. I dont know if it would evaporate out of the naptha in a crystal form like DMT though. So salting the water with tartric acid is used to salt LSA into LSA tartrate. maybe HCL, sulfate, or citrate would work too. I think that Dr. Hofmann back in the day might have made it more complicated then realized. LSD synth might be less complicated then it appears. If the crystals are impure in salt form then they can be washed like salvinorin crystals in naptha.

 

Ok what I have come to realize upon meditaion of this subject over the last few weeks is.

1. That a typical acid/base extraction with a crystal purifying step would produce pure LSA salt depending on the acid used.

2. That you would need 40,000 hbwrs or 1,000,000 mgs to make enough LSA extract for the recipe above.

3. 20mg LSA per 1kg of stipa robusta = 1,136lbs to get 10gs of LSA.

4. The best source is going to be from cultivated ergot.

 

Here in alt.drugs have been lot of talk about LSD synthesis lately.
I guess as an conclusion it can be said that the synthesis can be
carried out with good chemistry knowledge and laboratory. Then the
problem is where to get lysergic acid derivative for the synthesis.
The full synthesis of the lysergic acid is too difficult. Lysergic
acid amides can be extracted from the seeds of morning glory or
hawaiian baby wood rose, but it is not practical, because the huge
amount of seeds needed to get enough lysergic acid amides for
the LSD synthesis. To my opinion the only feasible possibility is
to cultivate ergot.
What I would like to know is how difficult it is to cultivate
Claviceps purpurea for example. Is it harder than growing psychedelic
mushrooms? Is the following procedure any good and how hard it is
to carry out? Any constructive comments?

Michael Valentine Smith: Psychedelic Chemistry
From pages 105-107:
The Culture and Extraction of Ergot Alkaloids
Make up a culture medium by combining the following ingredients in about
500 milliliters of distilled water in a 2 liter, small-neck flask:
Sucrose .......................................... 100 grams
Chick pea meal .................................... 50 grams
Calcium nitrate ..................................... 1 gram
Monopotassium phosphate ......................... 0.25 grams
Magnesium sulphate .............................. 0.25 grams
Potassium chloride ............................. 0.125 grams
Ferrous sulphate heptahydrate ................... 8.34 milligrams
Zinc sulphate heptahydrate ...................... 3.44 milligrams
Add water to make up one liter, adjust pH 4 with ammonia solution and
citric acid. Sterile by autoclaving.
Inoculate the sterilized medium with Claviceps purpurea under sterile
conditions, stopper with sterilized cotton and incubate for two weeks
periodically testing and maintaining pH 4. After two weeks a surface
culture will be seen on the medium. Large-scale production of the
fungus can now begin.
Obtain several ordinary 1 gallon jugs. Place a two-hole stopper in
the necks of the jugs. Fit a short (6 inch) glass tube in one hole,
leaving 2 inches above the stopper. Fit a short rubber tube to this.
Fill a small (500 milliliter) Erlenmeyer flask with a dilute solution
of sodium hypochlorite, and extend a glass tube from the rubber tube
so the end is immersed in the hypochlorite. Fit a long, glass tube in
the other stopper hole. It must reach near the bottom of the jug and
have about two inches showing above the stopper. Attach a rubber tube
to the glass tube as short or as long as desired, and fit a short glass
tube to the end of the rubber tube. Fill a large, glass tube (1 inch x
6 inches) with sterile cotton and fit 1-hole stoppers in the ends.
Fit the small, glass tube in end of the rubber tube into 1 stopper of
the large tube. Fit another small glass tube in the other stopper.
A rubber tube is connected to this and attached to a small air pump
obtained from a tropical fish supply store. You now have a set-up for
pumping air from the pump, through the cotton filter, down the long
glass tube in the jug, through the solution to the air space in the top
of the jug, through the short glass tube, down to the bottom of the
Erlenmeyer flask and up through the sodium hypochlorite solution into
the atmosphere. With this aeration equipment you can assure a supply
of clean air to the Claviceps purpurea fungus while maintaining a
sterile atmosphere inside the solution.
Dismantle the aerators. Place all the glass tubes, rubber tubes,
stoppers and cotton in a paper bag, seal tight with wire staples
and sterilize in an autoclave.
Fill the 1-gallon jugs 2/3 to 3/4 full with the culture medium and
autoclave.
While these things are being sterilized, homogenize in a blender the
culture already obtained and use it to inoculate the media in the
gallon jugs. The blender must be sterile. Everything must be sterile.
Assemble the aerators. Start the pumps. A slow bubbling in each jug
will provide enough oxygen to the cultures. A single pump can, of
course, be connected to several filters.
Let everything sit a room temperature (25 C) in a fairly dark place
(never expose ergot alkaloids to bright light - they decompose) for
a period of ten days.
After ten days adjust the culture to 1% ethanol using 95% ethanol
under sterile conditions. Maintain growth for another two weeks.
After total of 24 days growth period the culture should be considered
mature. Make the culture acidic with tartaric acid and homogenize in
a blender for one hour.
Adjust to pH 9 with ammonium hydroxide and extract with benzene or
chloroform/iso-butanol mixture.
Extract again with alcoholic tartaric acid and evaporate in a vacuum
to dryness. The dry material in the salt (i.e., the tartaric acid salt,
the tartrate) of the ergot alkaloids, and is stored in this form because
the free basic material is too unstable and decomposes readily in the
presence of light, heat, moisture and air.
To recover the free base for extraction of the amide of synthesis to
LSD, make the tartrate basic with ammonia to pH 9, extract with chloroform
and evaporate in vacuo.
If no source of pure Claviceps purpurea fungus can be found, it may be
necessary to make a field trip to obtain the ergot growths from rye or
other cereal grasses. Rye grass is by far the best choice. The ergot will
appear as a blackish growth on the tops of the rye where the seeds are
and are referred to as "heads of ergot." From these heads of ergot sprout
the Claviceps purpurea fungi. They have long steams with bulbous heads when
seen under a strong glass or microscope. It is these that must be removed
from the ergot, free from contamination, and used to inoculate the culture
media. The need for absolute sterility cannot be overstressed. Consult any
elementary text on bacteriology for the correct equipment and procedures.
Avoid prolonged contact with ergot compounds, as they are poisonous and
can be fatal.
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So with that said. when one of us can get around to growing ergot we will be closer then we think to LSD. the above synthesis is not as difficult as it seems. obtaining the chemicals needed for the synth are also not difficult to obtain with proper funding.

 

EaZy PeeZy LeMoN sQuEeZy!

 

Ive posted the cultivation method a few times..

(till I find It)

 

(-)negative.
As a teen I stumbled across a witchcraft book. This book gave clues to plants and fungus. Ergot moldy bread was mentioned. We cultured.
Simply take Rye bread and moisten it, sit in a dark place and wait. You might have better results with Rye Flour.
Black fungus will grow. This is and can and might be Ergot. If its more of a purple dark shade them it most likely is. It will be fuzzy, as you are culturing it you should remove any white funk with sterile tools.
Mix and re moisten it, in some more time it should blacken all the way through..
1/4 oz dry pulverized powder will do you, Mix with Lucky Charms cereal and you will not even know you ate it..
The visual effect are much more pronounced than LSA. as in the waving looking through a fish tank water type vision/ solid lines will wave(table edge; ect)..

More effective Ergot trips can be made from the pod themselves. You must culture them also.. Finding them in the wild is difficult, If you can find the rye grass then you can infect it yourself and hope for a cold damp climate change , Like FALL. when molds are more prone.
Infect Rye Grass with your bread mold culture. simply make a solution and spray it on. Cross your fingers....


If you smart enough to write all that other stuff, Youll know how to use this

 

Thank you. I have heard stories of letting rye grain or flour mold to obtain ergot.

 

help if you had your own green house. grew rye grass and infected it..
I saw ergot pods for sale once at this (eye of horus)store, but its been closed..

 

One day dreams of the farm will manifest. For now It looks like Im stickin with MGS for my LSA journeys. At least I have my san pedro extractions for my psychedelic journeys. Also I have discovered a very good cooking technique for psychedelic herbs as well as organic chemisty extractions. Now that I discovered that a/b extractions can get any alkaloid. I can just make my own. It will take 569lbs of MGS to get the 10g LSA needed for the synthesis above.

 

They say that stipa robusta has a high LSA content. But at 20mg per 1000g. It would take 1136lbs to obtain the 10g needed.

 

Argyreia nervosa contain about 0.3% ergot alkaloids in dry weight =
10g 350g seed

 

my bad that would be 35kg of seeds HBWR
and 100kg MG seeds

please correct me if im wrong

Argyreia nervosa WR contain about 0.3% ergot alkaloids


Ipomoea violacea MG contain about 0.1% ergot alkaloids, including ergotmetrine, chanoclavine and lysergol. These are all derivatives of Lysergic acid

 

sure i got the seeds you do the rest! heee I wanna be a chemist...

 

There's a good business idea for ya, selling WR
or maybe you and ancient powers can work something out lol