Lysergic Acid Diethylamide (LSD) Syntheses from "Recreational Drugs" by Professor Buzz Introduction

LSD is, without a doubt, the king of hallucinogens. It is rather difficult to make by total synthesis, but with the right starting materials (lysergic acid, ergotamine) it is as easy to produce as your average !" or amphetamine. I call it the king because of the awesome potency, the usual hallucinogenic dose being about #$$ to %$$ micrograms orally. he amphetamine D&' (S (), which is #$$ times more powerful than mescaline, re)uires a dose of * milligrams. his gives one gram of LSD the potential to contain %,$$$ to #$,$$$ doses. +ith an average of about ,,$$$ doses per gram, the street value (based on -* a hit) of one gram of LSD is -.$,$$$. LSD Synthesis /s with the rest of this book, I will deal only with the synthetic manufacture of drugs (LSD included). If you want to grow the ergot alkaloids that begin the total synthesis of LSD, then you will have to go to the 'erck Inde0 and look up the references to the operation. 'ichael 1. Smith2s book, (sychedelic "hemistry, has a section on growing "laviceps purpurea, which yield ergot compounds. his section is very complete and informative, but I think that you should also look up the dangers of growing this fungus before doing it, as it causes a type of gangrene that can kill you (not to mention making your arms and legs fall off) upon contamination of your body. /s 'r. Smith2s book states, this fungus is very temperamental, hard to obtain, even harder to grow and diffficult to work with. Smith2s book gives many references and many formulas that you will not see here, but which are of great interest in the making of all hallucinogens (not 3ust LSD). his does not make my book incomplete. &n the contrary, I have given more than enough information to make every ma3or type of drug. 'y book is not intended to cut in on Smith2s book sales. It is intended to give you information and formulas that Smith2s book lacks. +here he gives many different types of formulas, I give only the fast, simple and high yielding formulas. /lso, you will not see the same formula in both his and my book, unless it is a general method and not specific. +hat his book lacks, my book gives (e)uipment, methods, basic chemistry, a wider variety of types of different classes of drugs, glossary terms, easier to understand wordage, how to buy and make precursors, etc.). +hat my book lacks, his book gives (more variety of hallucinogenic formulas, cultivation of pot and ergot, tests for activity, etc.). I feel it would be a good idea to buy his book and try some of these harder formulas after learning the basics and practicing some of the formulas from my book, for complete understanding first. 4orgive me for wandering from the sub3ect of LSD synthesis. /s this first chapter of formulas is for psychedelics, I felt it necessary to e0plain the difference of the only other book of this type. If you are sharp, and have carefully read my chapter on buying precursors, you should be able to get lysergic acid from a supplier. 5e warned, that the D6/ must be informed of the purchase by the supplier, according to laws re)uiring them to do so. Lysergic acid can be made. 4ollowing is the general method to give you a very good idea of the procedure and chemicals involved. Synthesis of Lysergic /cid 5y reacting 78ben9oyl8.8(58carbo0yethyl)8dihydroindole (see :"S, .#*; (#<.#) for the

preparation of this compound) with thionyl chloride, followed by aluminum chloride gives #8 ben9oyl8*8keto8#,=,=a,.,%,*8he0ahydroben9indole. his is then brominated to give the %8bromo8 derivative, which is converted to the ketol8ketone by reacting with methylamine acetone ethylene ketol. his is then hydroli9ed by acid to yield the diketone and treated with sodium metho0ide to convert it to the tetracyclic ketone. /cetylate and reduce this ketone with sodium borohydride to get the alcohol, which is converted to the hydrochloride form, as usual. he above hydrochloride is treated with thionyl chloride in li)uid sulfur dio0ide, to produce an amorphous chloride hydro chloride, which is converted to the nitrile with sodium cyanide in li)uid hydrogen cyanide. 'ethanolysis then gives the ester of the nitrile. /lkaline hydrolysis of this last compound, followed by catalytic dehydrogenation in water using a deactivated >aney 7ickle catalyst (see :&". #., %** #<%;) gives dl8lysergic acid. otal Synthesis &f Lysergic /cid his is the easiest way to totally synthesi9e lysergic acid. here are other ways, but after reviewing other methods, I found this to be superior. It is )uite complicated and it takes good modern e)uipment. :/"S, ?;, .$;? (#<*,). .8Indolepropionic acid, <%.* g ($.* mole) is dissolved in ,$$ ml of water containing =$ g of 7a&!. he solution is mi0ed with #$$ g of >aney 7ickle catalyst and hydrogenated at room temp in a steel bomb at about .,*$$ psi until the uptake of hydrogen stops (about =$8.$ hours). 4ilter off the catalyst and wash it with a little water to remove the product that is clinging to it. /dd ;* ml of concd !"l acid to the filtrate, and cool. If your reduction is incomplete, you will now have unreacted starting material separate, and this must be removed by filtration. 5en9oylate the filtrate (the Schotten and 5aumann method is preferable), using =#$ ml of #= 7 7a&! #;$ ml of ben9oyl chloride. @eep the solution alkaline throughout the ben9oylation, and keep the temp below %$A" by cooling. +hen the ben9oyl chloride is fully reacted, the reaction mi0ture is cooled and acidified with .$$ ml of !"l acid. 4ilter the crude product by filtration, wash with water, and e0tract with four # liter portions of hot water. Separate, and crystalli9e the resulting syrupy product from a few volumes of methanol. 4ilter and wash with a little cold methanol to get a little over #$$ g that melts at #*#8#*.A. his is l85en9oyl8.8beta8 carbo0yethyl8=,.8dihydroindole. his can be purchased to eliminate this step. #85en9oyl8*8keto8#,=,=a,.,%,*,8he0ahydroben9indole. ##; g of the above product (#8ben9oyl8.858 carbo0yethyl8=,.8dihydroindole) is mi0ed with =$$ ml of pure thionyl chloride. his solution is allowed to stand for .$ min, then it is warmed gently for #*8=# min on a steam bath. 60cess thionyl chloride is completely evaporated with the temp maintained between ==8=,A" in vacuo. he crude acid chloride is dissolved in dry carbon disulfate. his solution is added, in a thin stream, to a well stirred suspension of =%$ g of aluminum chloride in #?*$ ml of carbon disulfate in a *,$$$ cc flask. 7oteB this must be done under a fume hood. / comple0 will separate and bog down the stirring device. !eat this mi0ture under reflu0 with stirring for # hour. Decompose this mi0ture by adding *$$ g of ice, =*$ ml of concd !"l acid, and *$$ ml of water, all while good stirring is continued. "ooling of this operation is affected by periodic distillation of the carbon disulfate in vacuo. /fter the decomposition is complete, any remaining carbon disulfate is removed completely in vacuo, and the product is e0tracted with = liters of ben9ene. he e0tract is washed well with *$$ ml of = 7 7a&! in three portions, and then with water. Dry (with the usual magnesium sulfate), and evaporate to a small volume in vacuo. /dd this small volume to several portions of ether to get the ketone to crystalli9e (add slowly), and filter, then wash with ether to get ;* g of pure title product, mpB #%,8#%?A". #85en9oyl8%8bromo8*8keto8#,=,=a,.,%,*8he0ahydroben9indole. / solution of the above indole (.$* g) in =,=$$ ml of glacial acetic acid is warmed to %$A". +hile the reaction is illuminated with a =*$ watt bulb, .*= g of pyridine hydrobromide perbromide is added in portions, over * min with shaking. he solution is then heated to ,$A and is held between there and **A" for .$ min. reat the mi0ture with carbon, and evaporate to a small volume in vacuo. he residue is taken up with

=,=$$ ml of chloroform, and wash this solution with several portions of water, dry as above, and concentrate in vacuo. "rystalli9e the residue from =,=$$ ml of *$C acetic acid and *$C ether to get =?$ g of title product that melts at #;$.*8#;#.*A". /nother crop can be obtained from concentrating the fltrates. DieldB .$ g of less pure product. #85en9oyl8=,=a,.,%8tetrahydro8%8methyl8=8methyl8#,.8dio0olan8=8yl8methyl8aminoben9indol8*8 (#!)one. / solution of the last indole product above (=?$ g) and .$? g of methylaminoacetone ethylene ketol in %,*$$ ml of dry ben9ene is reflu0ed for =# hours under a slow stream of nitrogen. he mi0ture is cooled and #*# g of methylaminoacetone ethylene ketol hydrobromide is filtered off. he filtrate is washed with ice water, then e0tracted with =.* liters of cold dilute !"l acid containing #*$ ml of the concd acid. he acid e0tracts are immediately added to an e0cess of ice cold dilute 7a&!. 60tract with # #iter of chloroform, dry over magnesium sulfate, treat with carbon and concentrate by evaporation in vacuo. he residual ketol8ketone is crystalli9ed from acetone to yield ==$ g, mpB #.*8#.,A". *8@eto8%878methyl878acetonylamino8#,=,=a,.,%,*8he0ahydroben9indole. =$ g of the above product is dissolved in a mi0ture of =*$ ml of concd !"l acid and =*$ ml of water, and the solution is kept under nitrogen for * days at .?A. "ool the mi0ture, treat with carbon, filter, and concentrate the filtrate in vacuo to a small volume. reat the residue with an e0cess of sodium bicarbonate, e0tract with cold chloroform, and remove the chloroform by evaporation in vacuo at room temp. he crude diketone is powdered, slurried with ?* ml of ben9ene8ether, and filtered. DieldB <.; g, mpB #$*8#$?A". <8keto8?8methyl8%,*,*a,,,,a,?,;,<8octahydroindolo8(%,.)iso)uinoline. =* g of the above product is mi0ed with **$ ml of absolute ethanol. Stir this mi0ture under nitrogen and cool to 8#*A with an e0ternal free9ing mi0ture. Sodium metho0ide is added (#? g) and the mi0ture is stirred for #$ min at 8#$ to 8#=A. "ool to 8=*A, and the product is filtered and washed (while still in the funnel) with cold ethanol and ether. +ithout e0posure to air the crude ketone is immediately slurried with a little ice water and filtered. +ash with ice water, ethanol, then ether (all cold) to yield #, g of product melting at #%*8#%?A. %8/cetyl8<8keto8?8methyl8%,*,*a,,,,a,?,;,<8octahydroindolo8%,.8)uinoline. =% g of the last product is added to ;$ ml of cold acetic anhydride. he mi0ture is held at =*A for about * min, then thoroughly cooled, filtered, and the product (a solid) washed with ether to yield =$.* g, mpB #,<8 #?$A. / second crop is obtained by concentrating the mother li)uor by evaporation. / mi0ture of the last product (#.$ g) and #$ g of palladium carbon (*C), in .* ml of 0ylene, is heated under reflu0 for % hours. he catalyst is filtered and e0tracted with hot methanol and chloroform. he combined e0tract filtrates and the initial filtrate are combined and evaporated in vacuo. he residue is recrystalli9ed from water to give $., g of a monohydrate product that melts at =**8=*,A. his product is called %8acetyl8%,*,*a,,8tetrahydro8<8hydro0y8?8methylindolo8(%,.fg)8 )uinolinium hydro0ide betaine. %8/cetyl8<8hydro0y8?8methyl8%,*,*a,,,?,;,<,#$8octahydroindolo8(%,.fg)8)uinoline. # g of the above betaine in a mi0ture of =$ ml of ethanol and * ml of water, is treated with $.$; g of sodium borohydride, and this solution is reflu0ed for #$ min and kept at =*A for # hour after the reflu0 is finished. he solvent is distilled off, and the residue is taken up in a mi0ture of chloroform and water. he chloroform solution is separated, dried as above, and then the solvent is distilled off. he residue is recrystalli9ed from a nitromethane8ethyl acetate mi0ture to yield $.= g (=#C), mp #<.8#<,A. 7ot only is this a small scale, but it is a poor yield, re)uiring you to perform it several times to get enough product to perform the ne0t step. +hen you have more than enough, convert the product into its hydrochloride form by dissolving in dry methanol and precipitating with dry hydrogen chloride.

%8acetyl8<8chloro8?8methyl8%,*,*a,,,,a,?,;,<8octahydroindolo8(%,.fg)8)uinoline hydrochloride. ..# g of the above product in its hydrochloride form is dissolved in ?* ml of li)uid sulfur dio0ide contained in a glass lined, high pressure bomb, or autoclave. hionyl chloride (#.= ml) is added and the vessel is sealed and kept at =*A for , hours. 1ent the vessel carefully and remove the mi0ture. 6vaporate the sulfur dio0ide while keeping the volume of the solution constant by the slow addition of dry ether. he amorphous chloro hydrochloride is filtered, washed with ether (dry) and dried by evaporating in vacuo to give ..* g of product, mpB#.$8#.*A. %8/cetyl8<8cyano8?8methyl8%,*,*a,,,,a,?,;,<8octahydroindolo8(%,.fg)8)uinoline. %$ g of dry, powdered sodium cyanide, is added to ice cold li)uid hydrogen cyanide and stirred gently with ice bath cooling. Speed up the stirring, continue the cooling, and add ?.* g of the amorphous product directly above. "ontinue stirring for .$ min, then the hydrogen cyanide is distilled under enough reduced pressure to keep it coming over the condenser at a temp below #$8#=A. he residue is mi0ed with chloroform and ice water, and the resulting mi0ture is filtered. he organic layer of the filtrate is separated and the a)ueous layer is e0tracted with two separate portions of chloroform. he combined e0tracts (this would include the separated chloroform, as usual) are dried over magnesium sulfate, decolori9ed, and the solvent removed by distillation in vacuo. "rystalli9e the product in ethyl acetate. DieldB ... g, mpB #?.8#?%A. >ecrystalli9e again for e0tra purity. <8"arbometho0y8?8methyl8%,*,*a,,,,a,?,;,<8octahydroindolo8(%,.fg)8)uinoline. # g of the last product is mi0ed with #* ml of methanol and $.=* ml of water. +ith e0ternal (ice bath) cooling add = ml of concd sulfuric acid slowly. Seal this solution in a high pressure bomb with a glass liner (or in a glass tube taking safety precautions in case of e0plosion) with a nitrogen atmosphere, and heat at #$$A for =.8=% hours. 7oteB I have seen a big pressure cooker (like gramma cans peas with) work for some of these bomb procedures. I do not recommend it, but here is how to do it right, if you feel you must. Ese only the great big heavy duty models, in e0cellent condition, set the pop off (relief valve) for near ma0imum positionF never, ever tamper or modify this valve to get more pressure. (ut the product in a glass beaker, put it in the cooker, flush with nitrogen, heat and stay in a different house during the reaction. "arefully turn off heat, notice or record pressure gauge after time has elapsed. +ait until pressure drops noticeably, bleed off remaining pressure and get product. reat the mi0ture with decolori9ing carbon and then evaporate in vacuo to #$ ml. (our onto a mi0ture of .$ ml of chloroform, ice, and #$ g of sodium bicarbonate. Separate the chloroform layer, and e0tract the a)ueous phase with three #$ ml portions of chloroform. he combined chloroforms are dried, evaporated to dryness in vacuo, and the product is crystalli9ed from ben9ene to give #G= g of product that melts at #*<8#,$A. Dou may purify more by recrystalli9ing from ethyl acetate. his is not very much product. /s with the procedure % steps back, you will have to perform this step over and over. If you try to double or triple the amounts given, you may get more product, but you will hurt the yield. dl8Lysergic acid. ..< g of the last product is mi0ed with ?; ml of #.*C potassium hydro0ide solution. >eflu0 for .$ min under nitrogen. ;.* g of hydrogen sodium arsonate, and >aney 7ickle (#, g wet), that has previously been deactivated by boiling in 0ylene suspension (see :&", %** (#<%;) to deactivate), is added and the mi0ture is reflu0ed and stirred under a nitrogen atmosphere for =$ hours. he solution is treated with carbon, and the crude lysergic acid is precipitated by neutrali9ation to p! *.,, and then filter it off and wash with water. DieldB #.$% g. / second crop is obtained in the usual manner ($.#* g). (urify by dissolving in dilute ammonium hydro0ide, treat with decolori9ing carbon, and reprecipitate with carbon dio0ide to get a mp of =%=8=%.A. Dou may be able to get an analytical or laboratory consultant to make one of these products near the final step, thereby eliminating the need to go through all of the steps as described. his will save you much time, but as these people are highly trained, their time will be costly. Lysergic acid can be made from many ergot derivatives by hydrolysis of these compounds. hese

compounds include ergonovine, ergotamine, ergokryptine, ergosine, methysergide, ergine, and a few others. otal synthesis of these compounds is impractical, as lysergic acid is made before the alkaloid. Dou could stop the operation as soon as you reach lysergic acid, otherwise you will have to hydroly9e as described below. here are many analogs of these alkaloids that end with the ine suffi0. hese are not as suspicious as the former because they lead to an inactive iso8LSD. hey will look like thisB the ergotamine isomer H ergotaminine, the ergonovine isomer H ergonovinine, etc. hese analogs are easily converted to the active forms or they may be used e0actly as the non8iso versions to give the iso8LSD, which is converted very easily to LSD as also described below. Lysergic /cid 4rom 6rgot /lkaloids. Dissolve =$ g of the alkaloid (use any of the above or one of its isomers or a combination) in =$$ ml of # ' methanolic @&! solution (this is made by dissolving #% g of @&! in =*$ ml of dry methanol) in a # #iter evaporation flask (heavy walled construction). 6vaporate the methanol off. /dd %$$ ml of ;C a)ueous (water) @&! solution to the residue and boil for one hour under a slow stream of nitrogen that is allowed to flow through a small orifice for e0hausting purposes. "ool, acidify with dilute sulfuric acid, and shake in a separatory funnel with # #iter of dry ether. Separate the lower a)ueous layer and filter it with vacuum assist. +ash the precipitate with =$ ml of dilute sulfuric acid. his is lysergic acidF store as described later in this chapter. here remains a small amount of lysergic acid in the filtrate solution. >emove it by basifying the solution with sodium carbonate, and then bubbling "&= through it. 4ilter it off and add it to the other lysergic acid. 7ow you will need to precipitate the iso8lysergic acid out and convert it. If you did not use any iso8alkaloid then you will have very little iso8lysergic acid, but it is still worth converting. If you used iso8alkaloid, this is a must. (recipitate the iso8lysergic acid by adding some #$C !7&., filter, add more portions until no more precipitate forms. "onvert it to lysergic acid by adding . ml of #$C @&! per every $.# g of iso8lysergic acid, heat on steam bath for # hour under a nitrogen atmosphere. (recipitate the changed lysergic acid by acidifying with glacial acetic acid. he total yield of this entire operation (including the iso change) is a little under #$ grams. /s stated earlier, you may use only iso8 alkaloid in the hydrolysis step above to get iso8lysergic acid which can be used in the synthesis of LSD to get iso8LSD, which can be changed to the active LSD as described later. 7oteB iso8LSD is not active. Some sources say that lysergic acid does not need to be purifed. I feel that everything should be purified. In the event that something should go wrong with the formula, you can immediately rule out impurities as the cause. /lso, impurities create unwanted byproducts which can be poisonous, creating dangers for the drug user. (urification of lysergic acid is very easy. Dissolve the acid in dilute ammonium hydro0ide, treat with decolori9ing carbon, reprecipitate (after filtering off and washing product from the carbon) with carbon dio0ide. "onvert iso8LSD to LSD. /dd *$ ml of ethanol and * ml of % 7 @&! per every gram of iso8LSD. Let this mi0ture stand for = hours at room temp. 6vaporate in vacuo to get the LSD. Separate iso8LSD from LSD. Dissolve the residue of the mi0ture of LSDs from the end of the formula in #=$ ml of ben9ene and %$ ml of chloroform. /dd tartaric or maleic acid to precipitate the LSD, filter off, add a little ether and put in refrigerator for several days to get a little more LSD, which is filtered off and added to the rest. 6vaporate the filtrate in vacuo to get the iso8LSD and convert as above. LSD from Lysergic /cid. his is based on the formula taken from "/, *$, #$;$.d (#<*,) Dissolve *.* g of dry lysergic acid in #=* ml of acetonitrile that has been cooled to 8#$A and cool further to 8=$A with an e0ternal free9ing mi0ture. /dd ;.; g of trifluoroacetic anhydride in ?* ml of

acetonitrile (this solution must be cooled to 8=$A before the addition). 5e careful making this addition, so as not to raise the temp, etc. Let stand at 8=$A until all the lysergic acid dissolves (about #G= hours). /dd ?., g of diethylamine (or analog) in #*$ ml of acetonitrile and allow to set at room temp in darkness for = hours. 6vaporate in vacuo to get the LSD, which can be separated from the iso8LSD as above. LSD 4rom Lysergic /cid his is taken from "/, *?, *<?< (#<,=). It is designed by !ofmann to give #8methyl8D8lysergic acid, and is modified to give LSD and iso8LSD. Dissolve $.*% g of lysergic acid in #$ ml of freshly distilled phosphorous o0ychloride, stir $.%= g of powdered, fresh phosphorous pentachloride. /llow to stand at room temp for = min, then at <$A for = min, then evaporate in vacuo. 60tract the residue with he0ane to give lysergic acid chloride hydrochloride. o save time you may e0tract the reaction mi0ture without evaporating. /dd =.* g of the hydrochloride to a cooled solution of ? ml of diethylamine (or analog) in =* ml of methylene chloride that is cooled to $A 7ote his solution is cooled to $A before the addition. +ith stirring add #..?* ml of dry pyridine and stir for .$ min with cooling to keep the temp at $A or a little below. +arm to room temp and continue the stirring for <$ min. 6vaporate in vacuo to get the LSDs. Separate as already described. LSD 4rom Lysergic /cid 'onohydrate his is, in my opinion, the best of all the methods. It was designed to be used to e0periment with different types of amines, so if you would like to substitute diethylamine with another amine this would be the best bet. It also gives good yields (*$C or better) and is very easy. he reference that gives it (:'", #,, *.= (#<?.)), also gives potency data for many lysergamides and many of their formulas. he reading is good, interesting, informative, and the method given below gives no useful amount of iso8LSD, so separation of that product is not necessary. 5oth method / and 5 were from :'", #,, *.=. 'ethod /. / slurry of ..#* g d8lysergic acid monohydrate (monohydrate means dry) and ?.. g of diethylamine (or $.# mole of similar amine) in #*$ ml of pure chloroform is heated to reflu0. /fter the lysergic acid is dissolved (a few min) cool the mi0ture down to where reflu0 has stopped by removing the heat. 5efore the mi0ture cools any further = ml of phosphorous o0ychloride is added at such a rate as to give reflu0 (about = min). /fter addition, reflu0 for %8* min further until an amber8colored solution results. "ool to room temp and wash the mi0ture with =$$ ml of # ' ammonium hydro0ide. he chloroform solution was dried with 'gS&% (this would have to be after separation), filtered, and concentrated by evaporation in vacuo under a temp of .;A (at no time let the temp go over %$A). he last traces of solvent are removed at =8* mm. Dissolve the residue in a minimum amount of methanol and acidify with freshly prepared solution of =$C maleic acid in methanol (not a)ueous) to precipitate the LSD in its maleate form. 4ilter the fluffy white needles, wash with cold methanol and air dry to get =.= g of LSD that re)uires no further purification. 'ethod 5. his is proven to be more effective for using substituted amines. 'i0 the following slurryF ..#* g of dry d8lysergic acid in #*$ ml of chloroform and reflu0 in a . necked flask. /s soon as you have the reflu0 ad3usted add ?.. g of diethylamine (or $.# mole of analog) in =* ml of chloroform and at the same time, from another addition funnel mounted in the opposite neck of the flask, add = ml of phosphorous o0ychloride so that both the additions begin at the same time. he additions should be timed so that they both finish after =8. min. @eep at reflu0 with gentle heating for another .8* min until a clear amber8colored solution results. "ool thesolution to room temp and finish the work up, as in method / directly above, to get = g of LSD maleate. /s in method /, this method gives very little or no iso8LSD, so don2t worry about removing that. Lysergic /cid 'onohydrate I put this formula in this book specifically for the two methods (/ and 5) directly above, however, lysergic acid monohydrate can be used on any of the LSD formulas with possible success. I feel this may be easier than the first method given at the beginning of this chapter.

Dissolve #?* g of @&! in #,?*$ ml of water in a flask of * liters volume e)uipped with a reflu0 condenser and a gas inlet tube. If a stirring device is not re)uired, it should be removed and the open neck stoppered. !eat the mi0ture to ;$A under a stream of nitrogen and add *$$ g of ergotamine tartrate. !old the temp at ;$A for = #G= hours with bubbling from the nitrogen filled gas inlet tube. (our the mi0ture into a * gallon polyethylene bucket (made from the same material as a plastic gas can) filled with about , liters of ice. (ut the bucket in a cooling mi0ture to cool below #$A. 7eutrali9e the mi0ture by adding cold dilute sulfuric acid to a congo red end point (p! %.=). Lysergic acid and potassium sulphate will be seen to precipitate. Let stand for =8. hours in the *8 #$A cooling mi0ture. 4ilter with vacuum assist, and let vacuo suck as dry as possible. 5reak up the filter cake and put in a = liter beaker. 'ake a solution from #*$ ml of li)uid ammonia and =.* liters of very cold dry denatured ethanol and add to the reaction mi0ture. Stir for # hour and filter. @eep the fltrate and treat the filter cake to #G= the ammonia ethanol mi0ture as above. his second e0tract is filtered and the cake is washed with =*$ ml of the ammoniacal ethanol mi0ture. "ombine the fitrates, and evaporate to total dryness with a strong vacuum and gently heating. Do not heat at too high of a temp. Scrape the product from the vacuum vessel and put into a mortar. 'i0 ##. ml of methanol with .; ml of water, and rinse the rest of the residue from the evaporation vessel and dump into the mortar with the rest of the product. he slurry in the mortar is ground up well and filtered. +ash the flter cake with #*$ ml of cold water and use vacuum to suck dry for # hour. 5reak up the filter cake and dry at ;$8;*A under a high vacuum to get about ,*8?* g of cream8white to gray8white powder. his is lysergic acid monohydrate. I think that if you dry the lysergic acid (obtained from the ergot alkaloids by hydrolysis as described earlier) it will also work in methods / and 5. his is how you dry lysergic acidB dry under high vacuum at #%$8#%*A for =8. hours. LSD 4rom 6rgot /lkaloids his was invented by !ofmann and is a superior method because you may proceed from the ergot alkaloids to LSD without isolating the lysergic acid. "/, *?, #=*,; (#<,=). /dd #.= g of ergotamine hydrochloride to % ml of anhydrous hydra9ine and heat # hour at <$A. /dd =$ ml of water and evaporate in vacuo, to get d8iso8lysergic acid hydra9ine. # g of the lysergic hydra9ine is powdered well and added to %$ ml of $.# 7 (ice cold) !"# acid. o this, cooled to $A, is added % ml of # 7 7a nitrite, with good stirring. &ver =8. min, add %$ ml of $.# 7 !"# acid to get p! to *. Let stand for * min, basify with # 7 7a!"&., e0tract with #$$ ml of ether, and then with *$ ml of ether. +ash the ether layer with water and dry, then evaporate in vacuo at #$A. Dissolve the resulting yellow a9ide in about * ml of diethylamine at $A and then heat in a metal bomb at ,$A for # hour. If a bomb is unavailable you may get by with heating for .8% hours at %*A in a vented flask under a nitrogen atmosphere. /lso, I would flush the bomb with nitrogen before sealing and heating. >emove heat after time elapses and let stand (after bleeding off pressure for bomb method) for = hours and evaporate in vacuo to get $.? g of LSD and $.#* g of iso8LSD. he iso8LSD will not do anything (good or bad) if consumed, so you may leave it in with the LSD. Dou may also separate it and convert it to LSD as in the formulas ahove. LSD 4rom Lysergic /cid :&", =%, .,; (#<*<) his is a simple method that gives good yields of LSD with very little (if any) iso8LSD. Dou will be re)uired to purchase sulfur trio0ide from /llied "hemical and Dye "orp (ask for Sulfan 5, or S&.), but this is not a suspicious chemical so ordering is not a problem. Sulfur trio0ide8Dimethylformamide comple0 (S&.8D'4). his is a reagent re)uired for this method of LSD production. / completely dry == liter flask (round bottom) in an ice cooling bath is fitted with a condenser, stirring device, addition funnel, then is filled with #$8## liters of D'4 (dimethylformamide) that has been freshly distilled under reduced vacuum. Ese drying tubes to protect the reaction from all moisture (including atmospheric moisture). = pounds of sulfur trio0ide (S&.) are then added, with a great deal of caution, over %8* hours with stirring, dropwise. he temp must be held between $A8*A during this addition. Stir for #8= hours after the addition until

some separated, crystalline S&.8D'4 comple0 has dissolved. Store in the dark in a suitable vessel, in a refrigerator for not more than . months. Epon storage, the comple0 will turn yellow and then orange. his is normal. /s long as it is less than .8% months, it is still good. his mi0ture gives a molarity of # (# ') and can be made using #G= or #G% of the amounts above to scale down the version, still giving a # ' solution. Lysergic /cid Diethylamide. / solution of ?.# g of lysergic acid monohydrate. /s with any of the formulas calling for the monohydrate, you may substitute dry or anhydrous lysergic acid in place of the lysergic acid monohydrate by using a smaller amount of the dry lysergic acid. I have found that dividing the amount of the monohydrate by the constant of #.# gives a close amount of dry lysergic to use, e.g., ?.# divided by #.# H ,.* g, to substitute in the formula. Likewise, the monohydrate can be figured into a formula calling for dry lysergic, ,.* times #.# H ?.# g. /lso, if a formula does not specify if the lysergic acid is to be dry, e.g., add $.*% g of d8lysergic acid, then always use dry or monohydrate as any water will kill the yield. Dry as stated above. /s a general rule dry your lysergic acid as soon as you plan to use it (because it collects !=& from air). # g of lithium hydro0ide hydrate in =$$ ml of methanol is prepared. Distill off the solvent (methanol) on a low temp steam bath under reduced pressure, or evaporate under vacuum. he resulting glass8 like lithium lysergate residue, is dissolved in %$$ ml dry dimethylformamide (D'4). =$$ ml of this D'4 is distilled off with #* mm pressure through a #= inch helices8packed fractional column. "ool the resulting solution to $A, and with stirring, )uickly add the S&.8D'4 solution (*$ ml of # '). he mi0ture is stirred with cooling for #$ min and #=*.$ mmol. of the desired amine is added (that would be <.$* g of diethylamine). he stirring and cooling are continued for #$ min after the amine addition, and then the reaction is decomposed by adding %$$ ml of water. /fter stirring thoroughly the reaction mi0ture is treated with a saturated solution of 7a"l. able salt and water are fine for this if the salt is not iodi9ed. Ese =$$ ml of the saturated solution on the reaction mi0ture. 60tract the amide (LSD) with repeated portions of ethylene dichloride. est for completeness of e0traction with 1an Erk test or hold e0tract under black light briefly and look for fluorescence as compared with non8e0tracted ethylene dichloride, or use any indole test. he combined e0tracts are dried (with 'gS&% as usual), and then evaporated under vacuo to a syrup. @eep the temp below at least room temp. Dissolve the residue in about ,$ ml of dry methanol, acidify with solid maleic acid, treat to turbidity with dry ether, and refrigerate for .8, hours to get colorless soft needles of LSD maleate which are filtered from the mother li)uor. 'ore crystals may be obtained by evaporating the mother li)uor in a cool, dark place under vacuum. hings o >emember +hen +orking +ith 6rgot /lkaloids, Lysergic /cid, /nd LSD hese compounds are very sensitive and even unstable. his means that the following steps must be taken to keep from ruining your compound or yield. /lways use red or yellow photographic dark room light bulbs during any step of LSD manufacture. Direct sunlight, electric filament, or fluorescent light bulbs (etc.) will hurt the above compounds. Dark room bulbs are cheap and are a must. @eep all forms of !=& out of the reaction. horoughly dry all the glass ware to be used. Ese a drying tube filled with anhydrous 'gS&% (calcium chloride reacts with amines in an unfavorable way and should not be used). I can2t be there to hold your hand and guide you through every step, so unless the formula says to add water, the drying tube should be in use, and after the water addition is over, the drying tube goes back on. his way the reaction is always protected even if it does not need to be. 5etter safe than sorry. /lso, if you2re not sure if you should use dry reagents, use dry reagents anyway. /lso dry the lysergic acid (as described above) and any other precursors in whatever drying process re)uired for that compound before use. Dry the finished LSD or even any intermediate along the way after you have completed the product. Likewise, dry an intermediate that you may have purchased from a chemical supplier. @eep o0idi9ing agents from these items. 6ven the o0ygen in the air can o0idi9e some of these compounds. he formula states that during some of the reactions above, an inert gas (nitrogen) must be used for an atmosphere inside the reaction vessel. 7itrogen can be obtained in small bottles (tanks) at a very reasonable fee, without any )uestions asked. 'ake sure you use a

regulator and introduce a slow stream into the vessel by way of a gas inlet tube or an e)uivalent. /lways flush the vessel before putting any reagents into it (flush the air out with nitrogen). I would use a nitrogen atmosphere from the very beginning of the formula to the very end, even if the formula did not specify its use. 1ery few of the above formulas call for a nitrogen atmosphere during evaporation, but I feel this may be bad for yield and or potency. LSD has many doses per gram, and if you lose #G= g because you were too cheap to use three dollars worth of nitrogen, you have lost about =,$$$ doses at -* a dose H -#$,$$$ of LSD wasted. 5etter safe than sorryI /lso, any precursors you make or buy should be stored in a nitrogen atmosphere, as should LSD. his can be done by poking a gas inlet tube into the vessel trust above or a little below the substance) flushing the air out with a moderate stream of nitrogen then )uickly reinstall the cap or stopper. he best way to store LSD is by producing it in the maleate form. his not only makes it resistant to o0idation, but it purifies it, too. Ese the procedure above (:&", =%, .,;, or "/, *?, *<?<) when you get to the last dry8and8evaporate8in8vacuo step, then treat the residue as specified. 7ever sub3ect these compounds to e0cessive heat, or any type of temperature warmer than the inside of your refrigerator. 6ven LSD maleate will decompose in e0cess heat, so store in a refrigerator. @eep evaporation procedures cooled. his will slow the evaporation process down, but that is better than losing the product. Some of the above formulas re)uire heat for a reaction. his is &k, but do not e0ceed the temp stated at any time and never heat longer than needed. /lso, nitrogen atmospheres are used during heating operation. Substituents LSD analogs (lysergic acid amides) can be prepared by substituting amines in place of diethylamine. he potency usually drops anywhere from ..C to ?*C depending on the substituent. Diethylamine is highly suspicious, and the substituent will produce a lysergamide that is most likely legal, as legislation has only singled out lysergic acid diethylamide. Little work has been done on the potency of substituted Iysergamides, so a little e0perimentation by you may be in order. (ersonally, I would like to try substituting a potent phenethylamine or phenylisopropylamine such as D&' (S () or %8bromo8=,*8dimetho0yamphetamine. If I could get a government grant, or maybe a grant from a ma3or pharmaceutical corporation, like Ep3ohn or Lilly, then I could play around with such e0periments. he following substituents give lysergamides with potencies as indicated in doses per gram (remember that LSD gives about ,,$$$ to <,$$$ doses)B 6thylpropylamine =,$$$ to *,$$$ 'orpholide ,$$ to =,$$$ 'ethylpropylamine ,$$ to #,$$$ Dipropylamine ,$$ to #,$$$ 'ethylethylamine %$$ to ,$$ Dimethylamine .$$ to %$$ (yrrolidide .$$ to %$$ /s a point of reference, D&' (S () is one of the most powerful amphetamines, at =$$ doses per gram. /t -* a line, its value is about * times =$$ H -#,$$$ a gram. 4or more info see :'", #,, *.= (#<?.). "laviceps purpurea is not the only place to get d8lysergic amides. he plant group of "onvolvulacea has been found to posses lysergic acid amides such as ergine and several others. hese "onvolvulacea type of plants do not cause the dreaded St. /nthony2s fire, as does claviceps purpurea, and as a matter of fact, they are hallucinogenic if eaten in large doses. "are must be taken that the seeds have not been treated with poison to discourage usage as a mind alterant, or treated with methyl mercury to prevent spoilage.

+hen these seeds are to be used for LSD syntheses, make sure to clean off the white layer that surrounds them by singeing or mild burning. /lso, ask for !awaiian >ose +ood, as these are the only ones that contain an appreciable amount of lysergic related compounds. hese compounds must be e0tracted as below, hydroly9ed (like ergotamine) as above, and then used in any of the formulas that re)uire d8lysergic acid or possibly used directly in the !ofmann hydra9ine methodF "/, *?, #=*,; (#<,=). hese seeds have very little amide, so you can plan on )uite a lot of work in the e0traction step. /ccording to /. !offer and !. &smond, the most amide plentiful species (+oodrose) has a minute . to , mg of amide per every gram of seed. his means that if you e0tract very thoroughly, you will re)uire a little over =$$ g of seeds to get # g of amide, which will be reduced further after hydrolysis to give you about $.* g of usable d8lysergic acid. 60tract as follows. (ulveri9e the seeds in a clean blender until they are a fine powder. (ut this powder into a beaker, add # #iter of petroleum ether to every <$$ to #$$$g of powdered seeds, stopper the beaker to prevent evaporation and let set for . days. 4ilter off the petroleum ether and let evaporate to make sure no amides were e0tracted (there should not be much, if any) from the ether. /dd # #iter of methanol (dry is best) and let soak for % days with vigorous shaking, now and then. 4ilter off the methanol and evaporate it under vacuo (vacuum speeds the process). In the meantime, add *$$ ml of fresh methanol to the powder and e0tract it again for . or % days. 4ilter as before and e0tract again with about .$$ ml of methanol. "ombine the residues of all e0tractions and hydroly9e.

%, "a=(=&; J ="& J %"l H "a(=&, J = "&= J = "a"l= "a(=&, J %"& J ;"l H = (&"l. J % "&= J "a"l= (>iban, ". r. <*, ##,#, #;;=)

6asy synthesis of (&"l.

I2ve been devouring the phosphorus chapter in :. +. 'ellor2s K"omprehensive treatise on inorganic and theoretical chemistryK (1ol. 1III), which provided me with the following procedure for synthesi9ing phosphoryl chlorideB K+hen (=&* is saturated with dry !"l, it becomes li)uid, and the li)uid, on distillation, gives off (&"l., and leaves a residue of !(&..K (p. <%%) and K(...) when (=&* is heated (...) with 7a"l, (&"l. is formed (...)K (p. <%*) If you2re not in the possession of any (=&*, the same reference saysB K+hen "a.((&%)= is heated with finely divided Si&=, "aSi&. and (=&* are produced.K (p. ?%=) he latter procedure is similar to the industrial (and historical) synthesis of phosphorus (and a constituent part of that process), as described in the phosphorus threadB httpBGGwww.sciencemadness.orgGtalkGviewthread.phpItidH,* /lsoB K he composition of bone8ash may be taken to be (=&* .<.*C, "a& *=.*C (...)K (p. ?.*) 7ow turn the calcium compounds to something that doesn2t react with the (&"l. on formation, and use the mi0 in one of the first couple procedures.

uote! ""hen P#$% is saturated &ith dry '(l) it becomes li*uid) and the li*uid) on distillation) gi+es off P$(l,) and lea+es a residue of 'P$,-" (.- /00)

1es that might be a neat tric2 but try heating calcium .hos.hate mi3ed &ith carbon in a combustion tube heated to 4%5 (elsius and run dry (hlorine throught the heated mi3- A mi3ture of .roducts should come o+er incuding P$(l,- 6ust redistill to .urify-

Another .ath &ould be con+erting calcium .hos.hate to .hos.hide &ith aluminum .o&der or carbon and heat the .hos.hide in dry chlorine at 755 (elsius to ma2e P(l,8his can be o3idized to the o3ychloride &ith .otassium chlorate-

you can still scrape red ( off tens of thousands of striker strips and make ("l*, then hydroly9e that to (&"l.. 5ut I would not call that easy. L6dited on ;G#=G=$$; by chloric#M

from wiki
+orld production e0ceeds one8third of a million tonnes.L*M (hosphorus trichloride is prepared industrially by the reaction of chlorine with a reflu0ing solution of white phosphorus in phosphorus trichloride, with continuous removal of ("l. as it is formed. (% J , "l= N % ("l. Industrial production of phosphorus trichloride is controlled under the "hemical +eapons "onvention, where it is listed in schedule .. In the laboratory it may be more convenient to use the less to0ic red phosphorus.L,M It is sufficiently ine0pensive that it would not be synthesi9ed for laboratory use.

boiling point

PCl3

76.1 C, 349 K, 169 F (reparation (hosphoryl chloride can be prepared by the reaction of phosphorus trichloride with o0ygen at =$O *$ A" (air is ineffective)B = ("l. J &= N = &H("l. /n alternative synthesis involves the reaction of phosphorus pentachloride (("l*) and phosphorus pento0ide ((%&#$). Since these compounds are both solids, a convenient way of performing the reaction is to chlorinate a mi0ture of ("l. and (%&#$, which generates the ("l* in situ. /s the ("l. is consumed, the (&"l. becomes the reaction solvent. , ("l. J , "l= N , ("l* , ("l* J (%&#$ N #$ (&"l. (hosphorus pentachloride also forms (&"l. by reaction with water, but this reaction is less easily controlled than the above reaction. POCl3 Boiling point

105. C !379.0 K"

#$% &'t($book )%* P$o+p$or,+ Bibl%

L 5ack to the "hemistry /rchive M 'aterialsB * Pallon 5ucket Drill (#G=K chuck) 'udG(aintG"oncrete 'i0er "offee 4ilters Strainer (big enough to fit over pot and bucket opening) = gallon "ooking (ot in Snips or Scissors =$$ 'atchbook 5o0es = Pallons /cetone Sulfuric /cid !ydrochloric /cid +ater Iodine

60tracting >ed (hosphorus from 'atchbooksB >ip off matchbook covers. Line up as many matchbook covers as you can cut through with tin snips or good, sharp scissors. "ut out and save all the striking strips. Drill .G%K hole in the lid of the * gallon bucket. (ut the mud mi0er through .G%K hole in lid and into the drill. Dump the =$$ matchbook bo0es worth of striking strips (#$,$$$ striking strips) into the * gallon bucket. (our #.* gallons of acetone into the bucket. "over bucket by inserting mud mi0er then snapping on the lid. 'i0 "ontents for about * minutes. "heck to see if strips are mostly white on account of the phosphorousGglue being washed off. If not then continue mi0ing. ake off the lid and pull out mi0er. (ut the strainer on the cooking pot and pour all the acetone in. (ull out all strips from strainer and bucket and place on clean table or in a bowl. he strips will be covered in residual red phosphorus, so rinse them by placing the strainer on bucket and throwing a handful of strips in it. hen slowly pour some of the acetone in the cooking pot, through the strainer until strips are clean. 6mpty strainer into garbage. "ontinue until all strips are rinsed. (our all the acetoneG>( into the cooking pot. Let the >( settle for about #* minutes. Slowly pour off the acetone. @eep pouring as long as the acetone is pretty clear. he last bit of acetone will be reddish colored. 4ilter this through a coffee filter in the strainer. Scrape the mushy >( back into the pot or dry the filters, roll and ball them up well, then unfold. /ll the >( will fall right out in a dust. "leaning 'atchbook >ed (hosphorusB SulfuricGhydrochloric acid washB ( his can be done as = different washes) +ith mushy >( in cooking pot, pour enough #B# waterGsulfuric to cover the glob. (It2s optional now to add heat or not. If so then add no more than enough for a light boil) 'i0 contents for * to #$ minutes. /dd an e)ual amount of hydrochloric acid and continue mi0ing for * to #$ minutes. If heat was applied take off now. /dd an e)ual amount of cold water. 4ilter through a coffee filter in the strainer. Scrape the chunky >( off the filters back into the cooking pot. ( his will eat up a lot of small paper fibers, hair, cotton, lint or whatever.) /cetone washB /dd enough acetone to cover the globs and chunks of >(. (/gain you can add heat if you like. 5ring it to a controlled boil.) 'i0 for * to #$ minutes. Let cool or add a little cold water. 4ilter >( same way and return it to pot. ( his will remove any glues or other acetone solvent 3unk.) +ater washB /dd enough distilled water to cover the >( globs. 5ring this to a boil for * to #$ minutes. 4ilter out the >( and leave in filters to dry out. +hen dry roll and ball up filters then brush out dust. "ollect dust in a baggie and store. ( his is a general cleaning to remove any chemical residue.) &ther washesB /ny of the following solvents have been safely used to wash >(... 'ethanol, 6thanol, Denatured alcohol, Isopropanol, oluene, Qylene. hese would be done the same as written above. ScreeningB (ut the >( in a stainless steel screen or plasticGsteel mesh style coffee filter and run acetone through it. he >( is washed through the screen with the acetone, and any particles larger than the screen apertures are filtered out. +ashing orderB he order does not matter as long as the >( is finished off with an acetone wash then a distilled water wash.

(refiring >ed (hosphorus >eact >(GI=B+eigh out your >( and put it into a bottle. /dd half as much I= to it and shake it up. /dd (dropwise) !=&= when not reacting. "ontinue shaking and adding drops of !=&= until it2s done reacting. 4ilter out >(B /fter prefiring add water and shake. If it won2t loosen up then put the bottle in boiling water for * minutes. 4ilter the waterG>(GI mi0. +ash the >( with acetone then water. Dry it out, baggie and save for a rainy day. 7oteB 'ake sure drill has a #G=K chuck. his was compiled from many sources and through trial and error was refined to what you see. It was written to be printed up and used as a reference for anyone like swim that hasn2t been able to get lab grade >(. Swim2s current run was scaled down using a = gallon bucket with ##% bo0esR It took over .G% gallon of acetone to e0tract the >(. "lean up will be !=S&%G!"l, acetone, !=&, prefire, acetone, !=&, doneR Swim is e0pecting to yield about =*$mg per bo0. hey2re hoping to end up with an even ounce.