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Synthesis of LSD-25 =================== This text was originally published in 1967 as The Psychedelic Guide to Preparation Eucharist by Robert E. Brown Preparatory arrangements ------------------------ Starting material may be any lysergic acid derivative, from Claviceps purpures (ergot) on rye grain or from culture, from Ipomea (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 is dissolved in 200ml of mathanoic KOH solution and the methanol removed immediately in vacuum. The residue is treated with 200ml of an 8% aqueous solution of KOH and the mixture heated on a steam bath for one hour. A stream of N2 gas is passed through the flask during heating and the evolved NH3 in the gas stream may be titrated in HCL to follow the reaction. The alkaline solution is made neutral to congo red with tartaric acid, filtered,cleaned by extracting with ether, the aqueous solution filtered and evaporated. Digest with MeOH to remove some of the colored material from the crystals of lysergic acid. Arrange the lighting in the laboratory similarly to that of a darkroom. Use photographic red and yellow safety lights since lysergic acid derivatives are decomposed by light. A weak, long wave ultraviolet source is conveniently made from the purple glass filter used in the 1950 ford dash lighting system. A small tungsten bulb will provide enough light. Have plenty of aluminum foil handy to cover reagents and products when light is present. Rubber gloves must be worn due to the highly poisonous nature of ergot alkaloids. A hair dryer, or, much 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 degrees C. The mixture is refluxed (or heated) for 30 minutes. With an open condenser, keep an inert atmosphere on the reaction. Add 1.5 volumes H2O and boil 15 minutes. On cooling in the refrigerator, isolysergic acid hydrazide is crystallized. Step II -Use Red Light Chill all reagents and have ice handy. Dissolve 2,82 g of the hydrazide rapidly in 100ml 0.1 N ice-cold HCL using an ice bath to keep the reaction vessel at o degrees. 100ml ice-cold 0.1 N NaNO2 is added and after 2 to 3 minutes vigorous stirring, 130ml more HCL is added dropwise with vigorous stirring again in an ice bath. After 5 minutes, neutralize 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 39ml ether extract. Allow to stand in dark, gradually warming up to 20 degrees 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 125ml of actonitrile and the suspension cooled to about minus 20 degrees C in a bath of acetone cooled with dry ice. To the suspension is added a cold -20 degrees C solution of 8.82 g of trifluoroacetic anhydride in 75ml of acetonitrile. The mixture is allowed to stand at -20 degrees C for about 1 1/2 hours during which time the suspended material dissolves, and the d-lysergic acid is converted to the mixture anhydride of lysergic and trifluoroacetic acids. The mixed anhydride can be separated in the form of an oil by evaporating the solvent in vacuum at a temperature below about 0 degrees C.Everything must be kept anhydrous. Step II - Use Red Light The solution of mixed anhydrides in acetonitrile from Step I is added to 150ml 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 vacuum, leaving a residue of LSD-25 plus other impurities. The residue is dissolved in 150ml of chloroform and 20ml 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 50ml portions of ice-water. The chloroform solution is then dried over anhydrous Na2SO4 and evaporated in vacuum. PREPARATION # 3 --------------- The following procedure gives good yield and is very fast with little iso-lysergic acid being produced, however, the stoichometry must be exact or yields will drop. Step I - Use White Light Sulfur trioxide id produced in an anhydrous state by carefully decomposing anhydrous ferric sulfate at approximately 480 degrees C. Store under anhydrous conditions. Step II - Use White Light A carefully dried 22 liter RB flask fitted with an ice bath,condenser, dropping funnel and mechanical stirrer is charged with 10 to 11 liters of dimethyformamide (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 with stirring, during 4 to 5 hours. The temperature is kept at 0-5 degrees 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 colorless may change to yellow and red, its efficiency remains unimpaired for three to four months in cold storage. An aliguot 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 L of MeOH is prepared. The solution is distilled on the steam bath under reduced pressure. The residue of glass-like lithium lysergate is dissolved in 400ml of anhydrous dimethyl formamide. From this solution about 200ml of the dimethyl formamide id distilled off at 15mm pressure through a 12- inch helices packed column. The resulting anhydrous solution of lithium lysergate left behind is cooled to 0 degrees and, with stirring, treated rapidly with 500ml 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 400ml of water is added to decompose the reaction complex. After mixing thoroughly, 200ml of saturated aqueous saline solution is added. The amide product is isolated by repeated extraction with 500ml portions of ethylene dicloride. The combined extract is dried and then concentrated to a syrup under reduced pressure. Do not heat the syrup during concentration. The LSD may crystallize 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 Long Wave UV The material is dissolved in a three to one mixture of benzene in chloroform. Pack a chromatography column with a slurry of basic alumina in benzene so that a one-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 50ml of solvent and 1 g LSD. Run this solution through the column, following the fastest moving blue fluorescent band. After it has been collected, strip the remaining material from the column by washing with MeOH. Use the UV light sparingly during this procedure to prevent excessive damage to the compounds. Evaporate the second fraction in vacuum and set aside for Step II. The fraction containing the pure LSD is concentrated in vacuum and the syrup will crystallize slowly. This material may be converted to the tartaric acid and the LSD tartrate conveniently crystallized. MP 190-196 Degrees 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. Neutralize with dilute HCl, make slightly basic with NH4OH and extract with chloroform or ethylene dicloride as in preparations #1 or #2. Evaporate in vacuum and chromatograph as in the previous step. Salvage ------- Neutralize all leftover solutions and residues with NaHCO3 and evaporate in vacuum to low volume. Extract with ammoniacal chloroform and evaporate the extract to dryness. This residue may be run through the whole process again and more LSD will be produced. Storage and use --------------- Lysergic acid compounds (among them LSD) 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 refrigerator. Packaging for use presents many possibilities, partially due to the incredibly small dosage involved. First a bio-assay of the solvent is made, then it may be measured by the volume of the solvent it is in. The solvent may be evaporated onto a weighed, calculated amount of some inactive powder such as chalk. sugar or baking soda. This bulky powder may be easily encapsulated in weightable portions. It is advantageous to add a trace of dry ascorbic acid to the dried powders. Sugar cubes offer a handy but extremely notorious method of dispensing. Other methods are without number, here being offered just a few occasionally used by the criminal element. Gelatin capsules are coated with the liquid solution and the capsules filled with an inert substance. Decoys such as this inert mixture might include a trace of brown color, a trace of quinine for fluorescence, and a trace of some relatively non-toxic compound which nearly mimicas the infra-red spectrum of LSD. For transport, a smuggler might evaporate a considerable amount onto a pocket handkerchief or onto a sheet of paper, providing the solution was properly decolorized before such treatment. These underhanded methods are used by criminals to avoid punitive action by law enforcement enthusiasts. One gram of pure LSD, if used in a truly enlightened, careful manner can be the door to a magnificent experience to nearly 3,000 individuals. Used furtively and in ignorance, the same amount may bring terrible confusion and abject terror to nearly one-third of these. BIBLIOGRAPHY ------------ Chem. Abstracts 44, 10740 Chem. Abstracts 38, 1499 c Chem. Abstracts 41, 2450 d JOC 24, 368 & 370 JBC 104, 547 Patent app. serial # 473, 443 by Eli Lilly Co. Dec. 6, 1954 =================================================================== Ergot Culture and Extraction of Lysergic Acid Derivatives ---------------------------- Claviceps purpures (Ergot) must first be isolated as a pure culture or obtained from a maintained collection of pure culture stocks. The culture is revitalized and prepared for inoculating a large culture by growing as a small surface culture on the medium described below for two weeks at ph 4. Sucrose........... 100 g Chick pea meal.... 50 g Ca (NO3)2......... 1.0 g Make up to 1 liter KH2PO4............ 0.25 g and adjust to ph 4 MgSO4............. 0.25 g with citric acid and KCL............... 0.125 g ammonia.Autoclave to FeSO4-7H2o........ 8.34 mg sterilize. ZnSO4-7H2o........ 3.44 mg Great care must be taken not to eontaminate the culture, since Claviceps is a parasite and is taken over by any number of more vigorous strains of saprophytic fungi and bacteria. Inoculate a number of large surface ferments in gallon jugs containing the above media, using the smaller culture by homogenizing it and using portions of it under sterile conditions. Prior to inoculation, make an aerator by ramming a large glass tube full of cotton,fitting one hole stoppers to the ends,attaching glass tubing,and attaching a stopper to fit the jugs with a vent tube to be extended to a flask containing a dilute solution of hypochlorite. Put the stoppers,tubing and filter in a paper bag stapled shut, and autoclave it. After inoculation, carefully place the assembled aerator on the jug and force air through it into the solution. Maintain aeration at 25 degrees in the absence of bright lights. After ten days, adjust the culture to 1 % ethanol using 95% ethanol (under sterile conditions), after which, growth is maintained under these conditions for 14 more days. The culture is made acidic with tartaric and is homogenized in a blender at maturity. After an hour, NH4OH is added to adjust the ph to 9.0 and the solution is extracted with benzene or chloroform isobutanol mixture. Extract with alcoholic tartaric acid and evaporate in a vacume to dryness. Recover the free base as needed by making the tartrate basic with ammonia to ph 9.0 and extracting with chloroform. Evaporate the chloroform in a vacume. Protect the base from light, heat, moisture and air. Extraction: Cultured ergot,ergot sclerotia,Morning glory seeds Equipment: Blender Separatory funnel Chromatography column Flash evaporator ( or hair dryer) Long wave UV lamp Reduce the material to a fine powder in a blender. if moist or wet, dry first, preferably in a vacume. Pack the powder in a large chromatography column as a slurry with ligroine or lighter fluid. Soak overnight and drip (percolate) slowly until the solvent is grease free. This takes about 5 oz./oz. of seeds, but less on ergot. When the fats are thus removed, an ammoniacal chloroform solution is washed slowly through. Prepare this solution by shaking 100ml con NH4OH in 900ml chloroform. The bottom chloroform layer is drawn off with the help of a separatory funnel. This chloroform wash should be dripped slowly through as soon as the ligroine fraction shows no grease film when evaporated in a watch glass. Collect and save the chloroform extract untilit doesn't fluoresce on evaporation of a drop on a watch glass. Evaporate this solution using a hair drier or even better, a flash evaporator. Wash the residue with a 3 % tartaric acid solution. Color the 3% tartaric solution with an acid-base indicator and estimate the number of moles of alkaloid present by titrating with this acid. Most of the residue should be dissolved or suspended. Transfer the solution to a separatory funnel,washing the evaporating vessel with extra acid. Make basic with NaHCO3 solution. Add equal volume of CHCL3. Shake thoroughly, let stand and remove the bottom layer. Extract again with chloroform. Reduce the combined chloroform extracts to a solid as before. Scrape the solid up with stainless steel spatula. This powder can be used directly to make the hydrazide. Ascorbic acid is usually used as a preserving agent. BIBLIOGRAPHY ------------ Chem. Abstracts 57, 13021 Chem. Abstracts 60, 11345 ===================================================================== Newsgroups: alt.drugs From: an40496@anon.penet.fi (Holden Caulfield) X-Anonymously-To: alt.drugs Organization: Anonymous contact service Reply-To: an40496@anon.penet.fi Date: Sat, 27 Nov 1993 23:07:53 UTC Subject: An amidation of lysergic acid. For anyone who's interested, here's another route for amidation of lysergic acid. I don't know if it's at all practical - what is phenyl N-phenyl- phosphorylamidochloride? I don't know what "amidochloride" means. Is it available, or cheap, and does it require special handling precautions? Will the reaction be air- or water- sensitive? It's not for my use, anyway. I am just posting it here for interest. From Chemical Abstracts 109: * * * 109:170694r Preparation of substituted amides of lysergic acid and its derivatives. Stuchlik, Josef; Cvak, Ladislav; Kejzlarova, Jana; Schreiberova, Magdalena; Krajicek, Alois; Cerny, Antonin. Czech. CS 246,643 (Cl. C07D457/06), 16 Nov 1987, Appl. 85/1,497, 04 Mar 1985; 5 pp. The title compounds I(R=HO, R3R2N; R1=H, C1-4 alkyl, 1-hydroxy-2- C2-4 -alkyl; R2=H,C1-2 alkyl; R3=C1-4 alkyl;R4=H,C1-4 alkyl) are prepared by reaction of acid I(R=OH) (II) in the presence of phenyl N-phenylphosphorylamidochloride (III) with amine HNR1R2 (IV). I are suitable for therapeutic applications. Lysergic acid (10 g) was suspended in 10 mL CH2Cl2, 10 mL Et3N are added, and the suspension mixed 10 minutes at room temperature. Then, 12 g III and 4 g (S)-(+)-2-amino-1-butanol were added. After 1 hour stirring, the reaction mixture was extracted with 5% NaOH solution and water. The organic phase was dried and concentrated by evaporation to give 12.5 g crude methylergometrin. COR | / \ || | || N-R3 / \\/ \ / || | | || | | \ //\ / | || R4-N--|| I * * * By the way, what routes are there for amidation of lysergic acid? I've heard of: - SO3-DMF (Garbrecht method - the best?) - trifluoroacetic acid - hydrazide (Stoll & Hofmann - the first) - acid chloride hydrochloride (Stoll & Hofmann; Garbrecht says acid chloride decomposes, but I think there are later reports using acid chloride hydrochloride. I think Experientia 17: 206-7 (1961) describes this, but I can't speak German, so I don't know. I'd type it in if someone would translate it) - using carbonyl diimidazole as dehydrating reagent - phenyl N-phenylphosphorylamidochloride method (this one) and there's an unusual LSD synthesis starting from elymoclavine (like lysergic acid except the COOH becomes CH2OH and the double bond is moved to next to where it is in lysergic acid) which uses MnO2 for in situ oxidation. ------------------------------------------------------------------------- To find out more about the anon service, send mail to help@anon.penet.fi. Due to the double-blind, any mail replies to this message will be anonymized, and an anonymous id will be allocated automatically. You have been warned. Please report any problems, inappropriate use etc. to admin@anon.penet.fi. ======================================================================== ---------------------------------- LYSERGIC ACID DIETHYLAMIDE ---------------------------------- GENERAL INFO ------------ 9,10-Didehydro-N,N-diethyl-6-methylergoline-8(beta)-carboxamide; N,N-diethyl-D-lysergamide; D-lysergic acid diethylamide. C20 H25 N3 O. US pat. 2,736,728; 2,774,763 (both in 1956 to Lilly); 3,141,887 (1964 to Farmitalia). First developed by Hoffman 1943. Melting point 80-85F. Soluble in water. STRUCTURE --------- C2 H5 \ _____ NOC / \ / \ || | C2 H5 _____ _____ // / \ / \----- | | | NH \ / \ / | - N - ------------ | CH3 CREATION PROCESS ---------------- LSD can be derived from the ergot alkaloids such as ergonovine, principal constituents of ergot, the grain deformity and toxic infectant of flour caused by the fungus of grasses, Claviceps purpurea. The microbial formation occurs over the hydroxyethylamide. LSD is produced by an anhydrous (water free) reaction between lysergic acid, trifluoroacetic acid, acetonitrile, and diethylamine. The reaction time for the entire process requires from 2 to 3 days. Lysergic acid is a psychomimetic under government control. Lysergic acid and isolysergic acid are the main cleavage products formed on alkaline hydrolysis of the alkaloids which are characteristic of ergot. Morning-glory seeds can be used as a source for lysergic acid, 1 kilogram (2.2 pounds) yields approximately 25 grams of lysergic acid amide which can be made to yield more than three grams of LSD. A solution of the mixed anhydride of d-lysergic acid (the levo [left]-rotating form is almost completely inactive and therefore useless as a starting material) and trifluoroacetic acid in 200 ml. of acetonitrile is obtained by reacting 5.36 grams of d-lysergic acid and 8.82 grams of trifluoroacetic anhydride. The mixture must be carefully handled so it doesn't pick up water from the air. Next, almost any diethylamine compound is dissolved in more acetonitrile and the two solutions are mixed. For all of these processes, the vessels must be stoppered with a water-absorbing salt such as calcium chloride to keep moisture out. However, after the initial mixture has reacted for 3 hours, water is deliberately added and it is shaken. Then, a solvent such as chloroform is added. The chloroform and water layers will separate, with nearly all of the LSD being in the chloroform layer. Pouring the LSD/chloroform mixture through a tube full of aluminum oxide will separate the two and the LSD will remain in the tube. ----------------------------------------------------------------------- HOW TO MAKE ************************** * * * + ++ ++ * * + / + + * * + +++ + + * * + / + + * * +++ ++ ++ * * * ************************** DOCS TYPED BY ShRxUd ------------------------------------------------------------------------- LSD : d-lysergic acid diethylamide ------------------------------------------------------------------------- OK This file is about LSD.. I will detail some methods of making it from chemicals and from seed.. It should be noted that this file is for informational purposes only.. :) :) HISTORY --------- LSD was first taken in its pure form by Dr. Albert Hoffman, a 37 year old Swiss chemist who worked at the Sandoz Pharmaceutical labs in Basel. In April 1943 he absorbed a drop of the 25th alkaloid solution (LSD-25) onto his finger by accident and noted that life had a "pleasant, fairy-tale quality". On April 19th he deliberatly swallowed some more, beginning with the tiny dose of 250 micrograms, or 25 millionths of a gram, a dose so small that no other drug known produces effects at these levels (200 micrograms is now considered a standard dose of LSD), and unbelivably to him he started tripping out.. Sandoz did further tests and these confirmed the enormous psychoactive potential for the drug.. The US army did huge experiments with LSD, testing it and its eight known deriatives as an incapitating agent for use in warfare, as well as testing it for possible uses in reversing brainwashing of soldiers.. There were secret tests done as well in which soldiers were unknowingly dosed and observed, also many were done in which they were knowingly dosed, and the films of these disorientated soldiers in a wartime situation were shown to demonstrate the great potential for LSD. Anyone outside the military can really only guess at the extent o f testing hidden from the public. The Russian scientists experimented with its warfare potential as well as parapsychological uses of LSD. The Weather Underground alledgedly held acid sessions to see if they had been infiltrated by an informer. The medica l profession also latched onto LSD, testing it for possible uses in rehablilitating psychotics and schitsofrenics with some positive results. Similar good results were recorded for people with heavy sex hang-ups, people addicted to drugs, and psychopaths. FORMS OF ACID --------------- ACiD is normally sold in trips, little blotter paper tabs about 1cm big although the size varies.. It can also be liquid, crystalline in powder form or in tablets of any description eg- microdots.. The standard dose is around 200 mics but the strength of the ACiD will vary enormously of course, as will the quality of the high. The diffent types of LSD eg (LSD-25, LSD-21, LSD mirror 21) all give vastly different trips and each one is of course variable. I think that the crystalline and the liquid forms are the purest. MAKING LSD ----- PT 1 - EXTRACTING LYSERGIC ACID FROM SEED ------------------------------------------- First get your seeds of preferably Woodrose (argyria [hawaiian baby woodrose]) variety but Convolvulaceae, Rivea, or Ipomoea will do.. The overall yield with this method is low, however it can be done with easily obtained chemicals.. NOTE - the following procedure requires some knowledge of lab techniques and unless you know what you are doing you could easily blow yourself up, or poison you and your friends if the final product is imperfect.. Proceed with caution.. --- Finely grind seeds and add NaHCO3. Extract with ethyl acetate by soaking about one day. Filter and extract the ethyl acetate with tartaric acid solution. Basify the extract with NaHCO3 and extract with ethyl acetate. Dry and evaporate the ethyl acetate to get the alkaloids. Repeat this procedure on the seeds until no more residue is obtained. This residue contains the natural alkaloids which are similar to LSD, as well as other plant products and impurities. Add 100ml petroleum ether to 100g finely ground seeds and let soak about two days. Filter, discard and let seeds dry. Add 100 ml methanol to the seeds let soak about two days. Filter, repeat extraction with another 100ml methanol and evaporate the methanol extracts in vacuum. This yellow residual oil contains the alkaloids. ERGOT ALKALOID HYDROLYSIS --------------------------- NOTE about ergot. In order to make LSD, lysergic acid is needed. This can sometimes be obtained, but generally one of the lysergic acid containing ergot alkaloids such as ergotamine is more readily available. Ergot is the dried sclerotium of various s pecies of fungi which infect rye (and other grasses) leading to the formation of large purple growths in place of the rye grains. These growths are collected,dried,powdered and the alkaloids extracted. Ergot is mainly produced in Europe (especially Switze rland). Some is grown in the USA, mainly for the use of ergotamine and related compounds in medicine (terminating migrane headaches etc) Many of the ergot alkaloids are deriatives (amides) of lysergic acid. Unfortunatly these compounds have little halluci nogenic activity and it is necessary to hydrolyze (split with water) off the amide, producing lysergic acid and to synthesise a different amide with greater psychadelic activity. This hydrolysis can be done with any of the following co mpounds or a mixture of them : ergometrine , ergine , ergotamine , ergosine , ergocristine , ergokrytine , ergonovine (ergometrine) , and methysergide (Sansert). When -ine is added to the name (eg- ergotaminine) this indicated the isomers which will produ ce inactive iso-LSD. A conversion process is detailed below. Dissolve 20mg of the alkaloid (previous extraction) in 200ml 1M KOH in methanol (ie. dissolve 56g KOH pellets in 1L 100% methanol) in a 1L heavy walled vacuum flask and evaporate the methanol in vacuum at room temperature. To prevent flask from cooling, thus prolonging the evaporation time place flask in a pan of water maintained at room temperature by gently heating or warm water running through. Add 400 ml 8% KOH in water to the residue and boil for one hour (under N2 if possible-this can be done by filling the flask with an N2 stream and loosely stoppering or by allowing a gently stream of N2 to flow through during heating. Cool, acidify with dilute sulfuric acid and shake in separatory funnel with 1L ether. Discard the upper ether layer and filter the aqueous suspension of lysergic acid(I) in vacuum. Wash precipitate with 20ml dilute sulfuric acid. To recover the small amount of (I) in solution remaining in solution, basify the Na carbonate and bubble CO2 through it. Filter and add precipitate to first batch. Some isolysergic acid will remain in solution and can be precipitated by adding 10% HNO3. It can be converted to (I) by adding 3ml 10% KOH for each 0.1g acid, boiling on steam bath for one hour under N2(if possible) and precipitating by acidifying with glacial acetic acid. Maximum yield is about 9g (I) for 20g ergotamine(alkaloid). PURIFYING ----------- About 20% of (I) will be isolysergic acid(non psychoactive) and it can be isomerized to (I) by the above procedure. Purifying is not nessecary but can be done to improve quality as follows.. Dissolve 9g (I) in 20ml NH4 OH, filter and concentrate in vacuum at room temperature to precipitate (I). After filtering, the grey crystals can be further purified by dissolving in boiling water and cooling in ice bath to precipitate (I). Melting point (point it decomposes at) is about 2400C Alternatively the dark coloured (I) resulting from hydrolysis can be shaken with 2 X 400ml 2 M NH4 OH in ethanol and the combined extracts evaporated in vacuum to give (I). Dissolve the remaining residue in 500 ml hot methanol, cool to 00C and filter out the (I). Coloured impurities can be removed by shaking solution with decolourizing carbon and filtering. MAKING LSD ------------ LSD FROM LYSERGIC ASID ------------------------ Dissolve 13.4g dry (I) in 250 ml dry dimethformamide and cool to 00C. Add cooled solution of 3.4 ml 0.35 M methanesulfonic acid anhydride in dry dimethylformamide. After thirty minutes at 00C add 14.6g (20.4 ml) diethylamine (DEA) and keep at 00C for o ne hour. Evaporate in vacuum to get LSD. Dissolve 5.3g dry (I) in 125 ml acentonitrile (or dimethylformamide or proprionitrile) and cool to -200C (freezer or dry ice-acetone or ethanol mixture). Add 8.82g trifluroacetic anhydride in 75 ml acetonitrile cooled to -200C carefully. Let stand at - 20 for 1= hours or until all (I) dissolves. Then add 7.6g DEA in 150ml acetonitrile and let stand at room temperature in dark two hours. Evaporate in vacuum to get LSD. Dissolve 0.536g (I) in 10 ml freshly distilled POCL3; stir and add 416mg powdered, freshly sublimed PCl5. Hold two minutes at room temperature, two minutes at 900C, and evaporate in vacuum. Extract the residue with hexane to give the lysergic acid chlo ride-HCl (can also extract the reaction mixture with hexane instead of evaporating in vacuum). Alternatively use 6ml POCl3 and 240 mg SOCl2 and heat three minutes at 900C to get the acid chloride. To 5g of the acid chloride add 1.4ml DEA in 50ml methane c hloride and cool to 00C. Stir and add 27.5 ml pyridine and stir = hour at 00 . Warm to room temperature and stir 1= hours. Evaporate in vacuum to get LSD. To a suspension of 13.4g dry (I) in 800ml dry dimethylformamide (DMF) in a 2L vacuum flask at 200, add a solution of 8.9g N,N'-carbonyldiimidazole in 250ml DMF and stir at 200 in dark for = hour. Add a solution of 4g DEA in 50ml DMF and let stand 2 hou rs at 200;then purify or dissolve residue in 2=L 2% tartaric acid; NH4OH and extract with a 9:1 solution of ether:ethanol. Dry and evaporate in vacuum to get LSD. Add 1L dimethylformamide (freshly distilled if possible) to dry flask fitted with stirrer, ice bath, dropping funnel and condenser, both protected from water by Ca chloride drying tubes. Add dropwise with stirring over 4-5 hours at 00 0.21bs (90.7g) So 3 (sulfuric anhydride, available as Sulfan from Allied Chem Co.) if precipitate forms, stir until it dissolves. Sulfan may be made in larger amounts and is good for several months if kept dry and cool. Molarity of fresh SO3-DMF reagant should be about 1M, but for precise determination add a little water to aliquot and titrate with standard NaOH to phenolphthalein end point. Add 6.45g dry (I) (or 7.15g (I) monohydrate) and 1.06 LiOH hydrate to 200ml methanolin a 1L vacuum flask and evaporate in vacuum. Dis olve residue in 400ml DMF at about 15mm Hg through a twelve inch column packed with glass helices or other material. Cool to 00 and rapidly add 50ml SO3-DMF solution (1 M). Stir at 00 for ten minutes and add 91.5g (12.9ml) DEA and stir ten minutes. Add 400ml water, stir and add 200ml saturated NaCl. Extract the LSD by shaking with several 500ml portions ethylene dichloride (can use indole test to show completeness of extraction). Combine extracts (lower layor in seporatory funnel) and dry, evaporate in vacuum to get LSD. To a reflexing slurry of 3.15g dry (I)(or monohydrate) in 150ml CHCl3 add 0.1 mole of the amine in 25ml CHCl3 and 2ml POCl3 simultaneously from seperate dropping funnels over 2 to 3 minutes. Reflux 3 to 5 minutes more till a clear amber solution result s. Cool to room temperature and wash with 200ml 1m NH4OH. Dry and evaporate in vacuum(below 400C). Can dissolve in the minumum amount of methanol. Filter and wash crystals with cold methanol and acidify with a fresh solution of 20% maleic acid in methanol . Filter and wash crystals with cold methanol to get the LSD or other amide. This method works with a wide variety of amines. For LSD itself, the POCl3 can be added first. The yield is about 50%. PURIFYING ----------- To purify your extracted LSD dissolve the residue in 150ml CHCl3 and add 20ml ice water. Pour into =L seperatory funnel and drain out the lower CHCl3 layer into a beaker (after shaking). Add 50ml CHCl3 to funnel, shake and drain bottom layer into same beaker. Repeat with 3 X 50ml CHCl3 and discard the water. Extract the combined CHCl3 extracts with 4 X 50ml ice cold water and dry, evaporate in vacuum the CHCl3 to get 3.5g d-LSD. This is composed partly of inactive d-iso-LSD which can be recovered and c onverted to d-LSD as follows: dissolve the residue in 120ml benzene and 40ml CHCl3 (or 200ml methanol), add tartaric or maleic acid and shake to precipitate mainly d-LSD (add a little ether and cool in refrigerator several days if nessecary to ensure comp lete precipitation)) Evaporate in vacuum the solvent to get d-iso-LSD. Ad 50ml ethanol and 5ml 4N KOH per g iso-LSD and let stand at room temperature for two hours, evaporate in vacuum (or extract with CHCl3 as above) to get LSD. SYNTHESING LSD ---------------- Another way to go about it is to synthesise LSD entirely as I will now detail. SYNTHESIS OF 2,3-Dihydrolysergic acid ----------------------------------- Condense methyl-6-methyl-nicotinate and 5-Br-isatin by fusion at 1800 to get 57% yield of (I) (I) in boiling glacial acetic acid is treated portionwise with powdered zinc and refluxed one hour to get (II). Treat (II) with NaBH4-BF3 (in ether) in tetrah ydrofuran as above to give (III) which when treated 24 hours with acetic anhydride gives (IV). Treat (IV) with methyl iodide in methanol-acetone in a Carius tube to get (V) which is reduced with KGH4 in aqueous methanol to get (VI). Treat (VI) with NH3 co ntaining NaNH2 for one hour to get 2,3-dihydrolysergic acid (VII) which can be converted to 2,3-dihydro-LSD which is about ten times less active than LSD. (VII) can be converted to lysergic acid prior to conversion to LSD, which will triple the yield in t erms of LSD activity. Dehydrogenation may work for the next process and also may work for converting 2,3-dihydro-LSD into LSD. LYSERGIC ACID FROM 2,3-Dihydrolysergic acid ------------------------------------------- To synthesise Lysergic acid from 2,3-dihydrolysergic acid dissolve 4g (VII) in 78ml 1.5% KOH and reflux five minutes (under N2 if possible). Add 8.5g Na arsenate hydrate and 16g Raney-Ni (wet [ deactivated by boiling in xylene suspension]) and reflux tw enty hours (N2 if poss). Filter, precipitate lysergic acid by taking pH to 5.6 with HCl; filter and wash precipitate with water to get 1g lysergic acid. Evaporate in vacuum the filtrate to get more product. NB: also see COMPLETE SYNTHESiS OF LSD for another method.. LSD VIA THE Hydrazide --------------------- Add 1.16g ergotamine.HCl to 4ml anhydrous hydrazine and heat one hour at 900. Add 20ml water and evaporate in vacuum. ( Purify by adding ether and aqueous tartaric acid, basify the aqueous phase and extract aqueous phase with CHCl3 to get mainly d-iso- lysergic hydrazide (I) ( Purify; chromatograph on alumina and elute with 0.5% ethanol in CHCl3)). To 1g (I),finely ground, in 40ml 0.1N ice cold HCl add with good stirring at 0W 4ml 1N Na nitrite. Quickly over 2-3 minutes add 40ml 0.1 N NaHCO3 and extract with 100ml ether, then 50ml ether. Wash ether with water and dry and evaporate in vacuum at 100.Dissolve the resulting yellow azide in about 5ml diethylamine(DEA) at 00 and heat one hour at 600 in a bomb(sealed metal pipe). Let stand several hours and ev aporate in vacuum to get about 0.7g d-LSD and 0.15g d-iso-LSD (convert as above). Alternativly the DEA can be added to the cooled ether solution of the azide and let stand several hours or overnight at room temperature in the dark in a vented flask. LSD IDENTIFICATION ------------------ There are a few ways to test for LSD presence and strength.. LSD fluoresces under an ultraviolet light (black light), but so do many other compounds. As LSD is an indole deriative it shows positive to these indole tests (which will also show DMT, psilocybe etc.) KELLER TEST Add a little of the powdered substance (0.2mg) to 1ml glacial acetic acid containing 0.5% FeCl3; layer underneath with 1ml concentrated sulfuric acid and shake. The colour varies with the indole. (Olive green - psilocin ; Red-Violet - psilocybin) VAN URK TEST Prepare Van Urk reagent by adding 0.5 g p-dimethylaminobenzaldehyde, 100ml water, 100ml concentrated sulfuric acid. Dissolve 1mg substanec in 1ml ethanol and mix with 2ml Van Urk reagent and illuminate for 10 minutes with an UV lamp (black light). (Psil ocin - blue-grey ; Psilocybin - red-brown) QUICK TEST Saturate strips of filter paper with a 2% p-dimethylaminobenzaldehyde in 45% ethanol; air dry and store in tightly stoppered amber bottles (or in dark), they will last several months. Put a little of the suspect substance in a few drops of ethanol (gin may do as a control), wet a filter paper strip in this and allow to dry. Put one drop concentrated HCl on the dried paper (dont let it touch anything). Alternativly, the powder can be placed directly on the strip and the HCl dropped on it. A violet red or violet blue indicates indole deriatives such as LSD. With DMT or psilocybin the colout is redder. The colour must be observed soon after adding the HCl as it rapidly changes. COMPLETE SYNTHESIS OF LSD --------------------------- Mix 32.8g (0.217M) methyl-6-methylnicotinate (other alkyl groups can replace either methyl group) with 45.2g(0.2M) 5-bromoisatin (apparently 4-Br or 4 or 5 Cl isatin will also work) in a 250ml flask at 1000 in an oil bath and raise the temperature to 1 700 and let react for 70 mins. Cool and then grind the solid as fine as possible in a mortar. Recrystallize from 150ml dimethylformamide and wash with ether to get 40g (57%) methyl-(5-bromo-3-isatylidene)-6-methyl-nicotinate (I). Suspend 10g(I) in 250ml g lacial acetic acid and heat to boiling. Add in small portions over 30 mins excess powdered zinc. Reflux one hour, filter and evaporate in vacuum and recrystallize the residue from dioxane to get 9.7g(95%) methyl(5-bromo-2-oxindol-3-yl)-6-methylnicotinate (II) to get a suspension of 18g dry NaBH4 in 300ml dry tetrahydrofuran add with stirring at 00 over 30 mins about 75g BF3 etherate. Stir 3 hours at 00, add 18g (II) and heat exactly 20 mins at precisely 22-240. Add carefully 150ml conc entrated HCl while cooli9!!!?gCC<<. Add 200ml water and stir 12 hours. Basify, extract the product with ethyl acetate and dry,evaporate in vacuum to get 11g of residue which recrystallizes from methanol to give methyl(2,3-dihydro-5-bromo-3-indolyl) -6-methylnicotinate (III) The following step may be unnessecary but it gives stability to (III). The acetyl group can be split off at the end of the synthesis, but is unnessecary since the 1-acetyl-LSD is as active as LSD. Treat 12g (III) at room temperature for 24 hours with acetic anhydride then hydrolyze and extract to get 11.5g residue which is ground in petroleum ether and recrystallized from cyclohexane (can chromatograph on alumina and elute with petroleum ether t o was out an oil, then with benzene containing 5% ethyl acetate to elute the product) to give methyl-(1-acetyl-2,3-dihydro-3-indolyl)-6-methylnicotinate (IV). Heat 5g (IV), 12.5ml acetone, 12.5ml methanol and 1.8ml methyl iodide for 18 hours in a Carius t ube at 700-800 C. Cool, filter, wash with acetone and recrystallize from methanol to get methyl-(1-acetyl-2,3-dihydro-5-bromo-3-indolyl)-1,6-dimethylnicotinate iodide (V). To 9.4g (V) in 250ml water and 250ml methanol at 350 add over 5 mins 2.9g KBH4 and stir 10 mins. Add 2.9g more KBH4 and stir 30 mins. Evaporate in vacuum and extract the residue with methylene chloride to get about 6.2g oily mixture containing about 2g of the d isomer (can seperate by chromatography if desired) of me thyl-(1-acetyl-2,3-dihyd9!!!?gCC<<lyl)-6-methyl-1,2,5,6-tetrahydronicot -inate (VI) To a suspension of finely powdered NaNH2 (6.1g) in 2 litres dry ammonia, add with stirring 8g (VI) in 50ml dry tetrahydrofuran. Stir one hour, add NH4Cl and evaporate the ammonia as fast as possible in a nitrogen stream. Extract at pH 8 with methylene chloride to get 6g (can chromatograph on 300g silica gel and 250g celite and elute with 98% benzene-2% absolute ethanol and evaporate in vacuum) or methyl-1-acetyl-2,3-dihydro-lysergate (VII) One method of dehydrating (VII) is above under LYSERGiC ACiD FROM 2,3-dihydrolysergic acid and another follows. Warm to dissolve 1.5g 2,3-dihydro-LSD in 5ml acetone, 40ml water and 40ml saturated NaHCO3. Cool to 200 and add all at once with vigourous stirring 2.46g potassium nitrosodisulfonate dissolved in 90ml water and 10ml saturates NaHCO3. After 1 min, extra ct 7 times with ethylacetate, wash the combined extracts with water, dry and carefully remove solvent to get a mixture of 12-OH-LSD, LSD and starting material which can be chromatographed to give about 0.2g 12-OH-LSD. The following method of converting (IV) to the diethylamide (which can probably be used in place of (IV) to give the diethylamide of (V), (VI) and (VII)) will probably also work admirably for (VII) or lysergic acid. Reflux 0.5g (IV) with 0.5 KOH in 30 ml methanol for 4 hours. Evaporate in vacuum and add water to the residue. Adjust the pH to between 5 and 6 and filter or centrifuge to get 0.3g of the free acid. Suspend 1.8g of the acid in 125ml chloroform, cool to minus 50 and add 0.5g triethylamine, then 0.6g ethylchloroformate and stir 45 mins. Add 2 ml diethylamine and stir 3 hours at room temperature to get, after the usual workup 1g of the diethylamide (recrystallize from benzene) OK I think thats about it.. Well I hope that covers it.. Where possible I have tried to include more than one method of doing things so if you dont have or cant get a particular chemical you can always try another method.. ============================================================================ Newsgroups: alt.psychoactives From: aankrom@blackfoot.ucs.indiana.edu (aankrom) Subject: References as promised... Message-ID: <Cnw8t4.HKG@usenet.ucs.indiana.edu> Date: Thu, 7 Apr 1994 14:41:27 GMT OK. The references that I mentioned, here they come... "Synthesis of Ergot Alkaloids from Tryptophan" J Rebek Jr., et al, JACS 106, 1813 (1984) "A New Synthesis of Lysergic Acid" eidem., Tet Lett 859 (1983) (and refs. therein.) "Emetic Activity of Reduced Lysergamides" FN Johnson et al, JMC 16, 532 (1973) (Lysergamides using s-amine and POCl3) I still feel like making a disclaimer that I am not encouraging this information to be used to synthesize illegal compounds, but for personal enlightenment. It's time to pull chem-wannabe's out of the Dark Ages! =========================================================================== Newsgroups: alt.drugs Distribution: world Subject: From the Merck Manual -- LSD references, etc Keywords: LSD, Lysergic Acid Amide, Lysergic Acid Summary: A couple of pages of copywrite infringement From the 11th Edition of the Merck manual, the "Centennial Edition" no less: [perhaps something to drop in the FAQ?] 5505. Lysergamide. 9,10-Didehydro-6-methylergoline- 8beta-carboxamide; lysergic acid amide; ergine. C16H17N3O; mol wt 267.32. C 71.88%, H 6.41%, N 15.72%, O 5.99%. Isoln from _Rivea_corymbosa_(L.) and from _Ipomoea_tricolor_ Cav., _Convolvulaceae_: Hofmann, Tscherter, _Experientia_ 16, 414 (1964). Prepn from lysergic acid hydrazide: Ainsworth, U.S. pat. 2,756,235 (1956 to Lilly); from lysergic acid and phosgene-dimethylformamide complex: Patelli, Bernardi, U.S. pat. 3,141,887 (1964 to Farmitalia). Microbiological production: Rutschmann, Kobel, U.S. pat. 3,219,545 (1965 to Sandoz). H. CONH2 '. / / \ / \ || | || N /\\ /\ / \ / \\ / \ / CH3 || | | \ || | | H \ // \ / \// \/ | || | || HN------- Prisms from methanol. dec 242deg. [alpha](5461)(20) + 15% (c = 0.5 in pyridine). Methanesulfonate, C7H21N3O4S, prisms from methanol + acetone, dec 232deg. Note: This is a controlled substance (depressant) listed in the U.S. code of Federal Regulations, Title 21 Part 1308.13 (1987). 5506. Lysergic Acid. 9,10-Didehydro-6-methylergoline- 8-carboxylic acid. C16H16N2O2; mol wt 268.32. C 71.62%, H 6.01%, N 10.44%, O 11.93%. Lysergic acid and isolyser- gic acid are the main cleavage products formed on alkaline hydrolysis of the alkaloids which are characteristic of ergot. Jacobs, Craig et al., _J._Biol._Chem._ 104, 547 (1934); 125, 289 (1938); 130, 399 (1939); 145, 487 (1942); _J._Org._Chem._ 10, 76 (1945). High-yield production by _Claviceps_paspali_: Arcamone et al., _Proc._Roy._Soc._ (London), _Ser._B_, 155, 26 (1961). total synthesis: Kornfeld et al., _J._Am._Chem._Soc._ 76, 5256 (1954); 78, 3087 (1956); M. Julia et al., _Tetrahedron_ _letters_ 1969, 1569; V.W. Armstrong et al., ibid. 1976, 4311; W. Oppolzer et al., _Helv._Chem._Acta_ 64, 478 (1981); R. Ramage et al., _Tetrahedron_ 37, Suppl. 9, 157 (1981); J. Rebek, D.F. Tai, _Tetrahedron_Letters_ 24, 859 (1983). Ste- reochemistry: Stoll et al., _Helv._Chem._Acta 37, 2039 (1954); Stenlake, _J._Chem._Soc._ 1955, 1626; Leeman, Fabbri, _Helv._ _Chim._Acta_ 42, 2696 (1959). Absolute configuration: Stad- ler, Hoffman, ibid. 45, 2005 (1962). H. COOH '. / / \ / \ || | || N /\\ /\ / \ / \\ / \ / CH3 || | | \ || | | H \ // \ / \// \/ | || | || HN------- Haxagonal scales, plates with one or two moles H20 from water, mp 240deg (dec). [alpha](D)(20) + 40deg (c = 0.5 in pyridine). Behaves as an acid and base, pKa 3.44, pKb 7.68. Moder- ately sol in pyridine. Sparingly sol in water and in neutral organic solvents; sol in NaOH, NH4OH, Na2CO3, and HCL solns. Slighly sol in dil H2SO4. Methyl ester, thin leaflets from benzene, mp 168deg. Note: This is a controlled substance (depressant) listed in the U.S. code of Federal Regulations, title 21 Part 1308.13 (1987). 5507. Lysergide. 9,10-Didehydro-N,N-diethyl-6-meth- ylergoline-8beta-carboxamide; N,N-diethyl-D-lysergamide; D- lysergic acid diethylamide; LSD; LSD-25; Lysergsaure Di- ethylamid. C20H25N3O; mol wt 323.42. C 74.27%, H 7.79%, N 12.99%, O 4.95%. Microbal formation by _Claviceps_pas- pali_ over the hydroxyethylamide; Arcamone et al., _Proc._ Roy._Soc._(London) 155B, 26 (1961). Partial synthesis: Stoll, Hofmann, _Helv._Chim._Acta_ 26, 944 (1943); 38, 421 (1955). Industrial prepn: Pioch; Garbrecht, U.S. pats. 2,736,728; 2,774,763 (both 1956 to Lilly); Patelli, Bernardi, U.S. pat. 3,141,887 (1964 to Farmitalia). Isotope-labeled LSD: Stoll et al., _Helv._Chim._Acta_ 37, 820 (1954). Toxicity data: E. Rothlin, _Ann._N.Y._Acad._Sci._ 66, 668 (1957). Review: Hof- fer, _Clin._Pharmacol._Ther._ 6, 183 (1965). Book: _The_Use_of_ LSD_in_Psychotherapy_and_Alcoholism_, H.A. Abramson, Ed. (Bobbs-Merrill, Indianapolis, 1967) 697 pp. / C2H5 H. CON '. / \ C2H5 / \ / \ || | || N /\\ /\ / \ / \\ / \ / CH3 || | | \ || | | H \ // \ / \// \/ | || | || HN------- Pointed prisms from benzene, mp 80-85 degs. [alpha](D)(20) + 17deg (c = 0.5 in pyridine). uv max (ethanol): 311 nm (E(1 cm)(1%) 257). LD50 in mice, rats, rabbits (mg/kg): 46, 16.5, 0.3 i.v. (Rothlin). D-Tartrate, C46H64N6O10, solvated, elongated prisoms from methanol, mp 198-200deg. [alpha](D)(20) + 30 deg. Soluble in water. Caution: This is a controlled substance (hallucinogen) listed in the U.S. Code of Federal Regulations, Title 21 Part 1308.11 (1987). USE: In biochemical research as an antagonist to serotonin. Has been used experimentally as adjunct in study and treat- ment of mental disorders. NOTES: Not guaranteed to be free from typos. Underlines are supposed to be italic (ie book/journal titles, etc) Alpha, beta, and deg are the greek letters and the degree symbol [alpha](D)(20) means a greek letter in [] followed by a subscript and then a superscript (I don't know *WHAT* this actually is) The chemical structures are almost exactly what the Merck manual has drawn. Almost nothing was lost in the conversion to ASCII. [if you wanted to get really technical, the lower hydrogen atom in all of the structures should be coming out, and have a thick line] ============================================================================= From: chadwell@utkvx.utk.edu Newsgroups: alt.drugs Subject: RE: Making LSD (or is that overstepping the bounds?) Date: Fri, 14 Oct 94 05:35:25 GMT Organization: University of Tennessee Lines: 53 Message-ID: <37m1f2$pj5@martha.utk.edu> References: ,<91018.gcochran@cat.ustanne.ns.ca> NNTP-Posting-Host: utkvx2.utk.edu Keywords: LSD, chemistry, synthesis In Article <91018.gcochran@cat.ustanne.ns.ca> "None O'Yours" <gcochran@cat.ustanne.ns.ca> writes: >As a complete idiot, and not intending to actualy try this, just how is >LSD made? How accessible are the ingredients? > >Just curious. > Contrary to popular belief, the synthesis of LSD (d-n,n-diethyl lysergic acid amide) or Delysid (the actual trade name) is not _that_ difficult. I does require some basic knowledge of laboratory organic chemistry, but nothing a few months of reading and practice can't accomplish (or a single semester of Organic Chem. at a college). The simplest procedure uses the Hoffmann Hydrazine Synthesis, which has some advantages and disadvantages. First, the disadvantages: It uses Hydrazine (NH2NH2), which is poisonous, highly flammable (it was originaly used as rocket fuel), and irritating. This converts racemic (read:both d & l) ergot alkoloids to lysergic acid hydrazide, as well as isomerizing them to the d-form (the l-form is inactive). The acid hydrazide is then reacted with acetyl acetone (2,4-pentanedione) to create lysergic acid pyrrazole. This product is then reacted with diethylamine to create the final product, which can then be made into the acid salt (bitartrate or ascorbate being the more common and well-known). I didn't go into detail, since as I said, this does require some basic lab knowledge. Hydrazine is dangerous stuff. Diethylamine is watched like a hawk by the DEA. The ergot alkoloids can be extracted from several sources, the most common being rye-smut (Claviceps pupurea, et. al.), Hawaiian baby woodrose seeds, or morning glory seeds. Throughout the procedure you use various solvents, some of which are flammable, toxic, or irritating. A fume hood is almost a certain requirement. So would be a non-sparking thermostaticly controlled hot-plate/stirrer. And a rotary evaporator really makes things much easier. There are other synthetic routes, (see Merck index, and others) but most of the others are difficult, long, dangerous (compared to the above, yeek!), and/or produce very small yields. As an example, one of them uses sulfur trioxide (SO3). This chemical is so hydroscopic (read: water-absorbing) that it will pull the water from wood so fast that it will char and likely combust! Also, H20+SO3 -> H2SO4 which is sulfuric acid. The fumes from this stuff are hideous. If you are really interested in these synthesis routes, hit the library and start looking up stuff in the "Chemical Abstracts", "Chemica Acta", and such. Look up the various chem-lingo so you know what it means (It took forever to find out just how to "bomb" catalyze....) +-----------------------------------+ + Leonard Chadwell, Jr. + Virtual Reality / TechnoMagick + aka - chadwell@utkvx.utk.edu + While - U - Wait ! + aka -phoenix@martha.utcc.utk.edu + Call for Estimates & Appointments. +-----------------------------------+ VR/TM Inc.