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Lysergic Acid Diethylamide (LSD) Synthesesfrom "Recreational Drugs" by ProfessorBuzz

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 youraverage !" or amphetamine. I call it the king because of the awesome potency, the usualhallucinogenic dose being about #$$ to %$$ micrograms orally. he amphetamine D&' (S),which is #$$ times more powerful than mescaline, reuires a dose of * milligrams. his gives onegram of LSD the potential to contain %,$$$ 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 (LSDincluded). If you want to grow the ergot alkaloids that begin the total synthesis of LSD, then youwill have to go to the 'erck Inde0 and look up the references to the operation. 'ichael 1. Smith2sbook, sychedelic "hemistry, has a section on growing "laviceps purpurea, which yield ergotcompounds. his section is very complete and informative, but I think that you should also lookup the dangers of growing this fungus before doing it, as it causes a type of gangrene that can killyou (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 anddiffficult to work with. Smith2s book gives many references and many formulas that you will notsee here, but which are of great interest in the making of all hallucinogens (not 3ust LSD). hisdoes not make my book incomplete. &n the contrary, I have given more than enough informationto 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 andformulas that Smith2s book lacks. +here he gives many different types of formulas, I give only thefast, simple and high yielding formulas. /lso, you will not see the same formula in both his and mybook, unless it is a general method and not specific. +hat his book lacks, my book gives(euipment, 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 mybook 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 harderformulas after learning the basics and practicing some of the formulas from my book, forcomplete 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 youare sharp, and have carefully read my chapter on buying precursors, you should be able to getlysergic acid from a supplier. 5e warned, that the D6/ must be informed of the purchase by thesupplier, according to laws reuiring them to do so. Lysergic acid can be made. 4ollowing is thegeneral method to give you a very good idea of the procedure and chemicals involved.

Synthesis of Lysergic /cid

5y reacting 78ben9oyl88(58carbo0yethyl)8dihydroindole (see :"S, #*; (#

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preparation of this compound) with thionyl chloride, followed by aluminum chloride gives #8ben9oyl8*8keto8#,=,=a,,%,*8he0ahydroben9indole. his is then brominated to give the %8bromo8derivative, which is converted to the ketol8ketone by reacting with methylamine acetone ethyleneketol. his is then hydroli9ed by acid to yield the diketone and treated with sodium metho0ide toconvert it to the tetracyclic ketone. /cetylate and reduce this ketone with sodium borohydride toget the alcohol, which is converted to the hydrochloride form, as usual.

he above hydrochloride is treated with thionyl chloride in liuid sulfur dio0ide, to produce anamorphous chloride hydro chloride, which is converted to the nitrile with sodium cyanide in liuidhydrogen cyanide. 'ethanolysis then gives the ester of the nitrile. /lkaline hydrolysis of this lastcompound, followed by catalytic dehydrogenation in water using a deactivated >aney 7icklecatalyst (see :&". #, %** #

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=,=$$ ml of chloroform, and wash this solution with several portions of water, dry as above, andconcentrate in vacuo. "rystalli9e the residue from =,=$$ ml of *$C acetic acid and *$C ether toget =?$ g of title product that melts at #;$.*8#;#.*A". /nother crop can be obtained fromconcentrating the fltrates. ieldB $ 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 methylaminoacetoneethylene ketol in %,*$$ ml of dry ben9ene is reflu0ed for =# hours under a slow stream ofnitrogen. he mi0ture is cooled and #*# g of methylaminoacetone ethylene ketol hydrobromide isfiltered off. he filtrate is washed with ice water, then e0tracted with =.* liters of cold dilute !"lacid containing #*$ ml of the concd acid. he acid e0tracts are immediately added to an e0cessof ice cold dilute 7a&!. 60tract with # #iter of chloroform, dry over magnesium sulfate, treat withcarbon and concentrate by evaporation in vacuo. he residual ketol8ketone is crystalli9ed fromacetone to yield ==$ g, mpB #*8#A".

*8@eto8%878methyl878acetonylamino8#,=,=a,,%,*8he0ahydroben9indole. =$ g of the aboveproduct is dissolved in a mi0ture of =*$ ml of concd !"l acid and =*$ ml of water, and thesolution is kept under nitrogen for * days at ?A. "ool the mi0ture, treat with carbon, filter, andconcentrate 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 atroom temp. he crude diketone is powdered, slurried with ?* ml of ben9ene8ether, and filtered.ieldB

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%8acetyl8

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compounds include ergonovine, ergotamine, ergokryptine, ergosine, methysergide, ergine, and afew others. otal synthesis of these compounds is impractical, as lysergic acid is made before thealkaloid. ou could stop the operation as soon as you reach lysergic acid, otherwise you will haveto hydroly9e as described below. here are many analogs of these alkaloids that end with the inesuffi0. hese are not as suspicious as the former because they lead to an inactive iso8LSD. heywill 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 thenon8iso versions to give the iso8LSD, which is converted very easily to LSD as also describedbelow.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 drymethanol) in a # #iter evaporation flask (heavy walled construction). 6vaporate the methanol off.

/dd %$$ ml of ;C aueous (water) @&! solution to the residue and boil for one hour under aslow 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 aueous layer and filter it with vacuum assist. +ash the precipitate with =$ mlof 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 thesolution with sodium carbonate, and then bubbling "&= through it. 4ilter it off and add it to theother lysergic acid. 7ow you will need to precipitate the iso8lysergic acid out and convert it. If youdid not use any iso8alkaloid then you will have very little iso8lysergic acid, but it is still worthconverting. If you used iso8alkaloid, this is a must.

recipitate the iso8lysergic acid by adding some #$C !7&, filter, add more portions until nomore precipitate forms. "onvert it to lysergic acid by adding ml of #$C @&! per every $.# g ofiso8lysergic acid, heat on steam bath for # hour under a nitrogen atmosphere. recipitate thechanged lysergic acid by acidifying with glacial acetic acid. he total yield of this entire operation(including the iso change) is a little under #$ grams. /s stated earlier, you may use only iso8alkaloid in the hydrolysis step above to get iso8lysergic acid which can be used in the synthesis ofLSD to get iso8LSD, which can be changed to the active LSD as described later. 7oteB iso8LSD isnot active.

Some sources say that lysergic acid does not need to be purifed. I feel that everything should bepurified. In the event that something should go wrong with the formula, you can immediately ruleout impurities as the cause. /lso, impurities create unwanted byproducts which can bepoisonous, creating dangers for the drug user. urification of lysergic acid is very easy. Dissolvethe acid in dilute ammonium hydro0ide, treat with decolori9ing carbon, reprecipitate (after filteringoff 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 theformula in #=$ ml of ben9ene and %$ ml of chloroform. /dd tartaric or maleic acid to precipitatethe 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 andconvert as above.

LSD from Lysergic /cid. his is based on the formula taken from "/, *$, #$;$d (#

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acetonitrile (this solution must be cooled to 8=$A before the addition). 5e careful making thisaddition, so as not to raise the temp, etc. Let stand at 8=$A until all the lysergic acid dissolves(about #G= hours). /dd ?. g of diethylamine (or analog) in #*$ ml of acetonitrile and allow to setat room temp in darkness for = hours. 6vaporate in vacuo to get the LSD, which can beseparated from the iso8LSD as above.LSD 4rom Lysergic /cid

his is taken from "/, *?, *

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Dissolve #?* g of @&! in #,?*$ ml of water in a flask of * liters volume euipped with a reflu0condenser and a gas inlet tube. If a stirring device is not reuired, it should be removed and theopen neck stoppered. !eat the mi0ture to ;$A under a stream of nitrogen and add *$$ g ofergotamine tartrate. !old the temp at ;$A for = #G= hours with bubbling from the nitrogen filled gasinlet tube. our the mi0ture into a * gallon polyethylene bucket (made from the same material asa plastic gas can) filled with about liters of ice. ut the bucket in a cooling mi0ture to cool below#$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#$A cooling mi0ture. 4ilter with vacuum assist, and let vacuo suck as dry as possible. 5reak upthe filter cake and put in a = liter beaker. 'ake a solution from #*$ ml of liuid 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. hissecond 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. Donot 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 evaporationvessel and dump into the mortar with the rest of the product. he slurry in the mortar is ground upwell 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 ofcream8white to gray8white powder. his is lysergic acid monohydrate.

I think that if you dry the lysergic acid (obtained from the ergot alkaloids by hydrolysis asdescribed earlier) it will also work in methods / and 5. his is how you dry lysergic acidB dryunder 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 theergot alkaloids to LSD without isolating the lysergic acid. "/, *?, #=*; (#

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some separated, crystalline S&8D'4 comple0 has dissolved. Store in the dark in a suitablevessel, in a refrigerator for not more than months. Epon storage, the comple0 will turn yellowand then orange. his is normal. /s long as it is less than 8% months, it is still good. his mi0turegives a molarity of # (# ') and can be made using #G= or #G% of the amounts above to scale downthe version, still giving a # ' solution.

Lysergic /cid Diethylamide. / solution of ?.# g of lysergic acid monohydrate. /s with any of theformulas calling for the monohydrate, you may substitute dry or anhydrous lysergic acid in placeof the lysergic acid monohydrate by using a smaller amount of the dry lysergic acid. I have foundthat dividing the amount of the monohydrate by the constant of #.# gives a close amount of drylysergic to use, e.g., ?.# divided by #.# H .* g, to substitute in the formula. Likewise, themonohydrate can be figured into a formula calling for dry lysergic, .* times #.# H ?.# g. /lso, if aformula does not specify if the lysergic acid is to be dry, e.g., add $.*% g of d8lysergic acid, thenalways use dry or monohydrate as any water will kill the yield. Dry as stated above. /s a generalrule dry your lysergic acid as soon as you plan to use it (because it collects !=& from air). # g oflithium hydro0ide hydrate in =$$ ml of methanol is prepared. Distill off the solvent (methanol) on alow temp steam bath under reduced pressure, or evaporate under vacuum. he resulting glass8like lithium lysergate residue, is dissolved in %$$ ml dry dimethylformamide (D'4). =$$ ml of thisD'4 is distilled off with #* mm pressure through a #= inch helices8packed fractional column. "oolthe 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 (thatwould be

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regulator and introduce a slow stream into the vessel by way of a gas inlet tube or an euivalent./lways flush the vessel before putting any reagents into it (flush the air out with nitrogen). I woulduse a nitrogen atmosphere from the very beginning of the formula to the very end, even if theformula did not specify its use. 1ery few of the above formulas call for a nitrogen atmosphereduring evaporation, but I feel this may be bad for yield and or potency. LSD has many doses pergram, 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 sorry

/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 thesubstance) flushing the air out with a moderate stream of nitrogen then uickly reinstall the cap orstopper. he best way to store LSD is by producing it in the maleate form. his not only makes itresistant to o0idation, but it purifies it, too. Ese the procedure above (:&", =%, ;, or "/, *?,*

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+hen these seeds are to be used for LSD syntheses, make sure to clean off the white layer thatsurrounds them by singeing or mild burning. /lso, ask for !awaiian >ose +ood, as these are theonly ones that contain an appreciable amount of lysergic related compounds. hese compoundsmust be e0tracted as below, hydroly9ed (like ergotamine) as above, and then used in any of theformulas that reuire d8lysergic acid or possibly used directly in the !ofmann hydra9ine methodF"/, *?, #=*; (#

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%,"a==&; J ="& J %"l H "a=& J = "&= J = "a"l="a=& J %"& J ;"l H = &"l J % "&= J "a"l=(>iban, ". r.

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6asy synthesis of &"l

I2ve been devouring the phosphorus chapter in :. +. 'ellor2s K"omprehensive treatise oninorganic and theoretical chemistryK (1ol. 1III), which provided me with the following procedure forsynthesi9ing phosphoryl chlorideB

K+hen =&* is saturated with dry !"l, it becomes liuid, and the liuid, on distillation, gives off&"l, and leaves a residue of !&.K (p.

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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 Pl,-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.

6dited on ;G#=G=$$; by chloric#M

from wiki

+orld production e0ceeds one8third of a million tonnes.*M hosphorus trichloride is preparedindustrially by the reaction of chlorine with a reflu0ing solution of white phosphorus in phosphorustrichloride, 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 usethe less to0ic red phosphorus.M It is sufficiently ine0pensive that it would not be synthesi9ed forlaboratory 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*) andphosphorus pento0ide (%$). Since these compounds are both solids, a convenient way ofperforming the reaction is to chlorinate a mi0ture of "l and %$, 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 easilycontrolled than the above reaction.

POCl3

Boiling point

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105. C !379.0 K"

#$% &'t($book )%* P$o+p$or+ Bibl% 5ack to the "hemistry /rchive M'aterialsB* Pallon 5ucketDrill (#G=K chuck)'udGaintG"oncrete 'i0er"offee 4iltersStrainer (big enough to fit over pot and bucket opening)= gallon "ooking otin Snips or Scissors

=$$ 'atchbook 5o0es= Pallons /cetone

Sulfuric /cid!ydrochloric /cid+aterIodine

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60tracting >ed hosphorus from 'atchbooksB

>ip off matchbook covers. Line up as many matchbook covers as you can cut through with tinsnips 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 andinto the drill.

Dump the =$$ matchbook bo0es worth of striking strips (#$,$$$ striking strips) into the * gallonbucket. our #.* gallons of acetone into the bucket. "over bucket by inserting mud mi0er thensnapping on the lid. 'i0 "ontents for about * minutes. "heck to see if strips are mostly white on account of thephosphorousGglue 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 acetonein. ull out all strips from strainer and bucket and place on clean table or in a bowl. he strips willbe covered in residual red phosphorus, so rinse them by placing the strainer on bucket andthrowing 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 arerinsed. our all the acetoneG> into the cooking pot. Let the > settle for about #* minutes. Slowlypour off the acetone. @eep pouring as long as the acetone is pretty clear. he last bit of acetonewill be reddish colored. 4ilter this through a coffee filter in the strainer. Scrape the mushy > backinto the pot or dry the filters, roll and ball them up well, then unfold. /ll the > will fall right out in adust.

"leaning 'atchbook >ed hosphorusB

SulfuricGhydrochloric acid washB (his can be done as = different washes) +ith mushy > incooking 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 aneual amount of hydrochloric acid and continue mi0ing for * to #$ minutes. If heat was appliedtake off now. /dd an eual 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 paperfibers, hair, cotton, lint or whatever.)

/cetone washB /dd enough acetone to cover the globs and chunks of >. (/gain you can addheat if you like. 5ring it to a controlled boil.) 'i0 for * to #$ minutes. Let cool or add a little coldwater. 4ilter > same way and return it to pot. (his will remove any glues or other acetonesolvent 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 thenbrush out dust. "ollect dust in a baggie and store. (his is a general cleaning to remove anychemical 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 runacetone through it. he > is washed through the screen with the acetone, and any particleslarger than the screen apertures are filtered out.

+ashing orderBhe order does not matter as long as the > is finished off with an acetone washthen a distilled water wash.

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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 it2sdone reacting.

4ilter out >B /fter prefiring add water and shake. If it won2t loosen up then put the bottle in boilingwater 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. Itwas written to be printed up and used as a reference for anyone like swim that hasn2t been ableto get lab grade >. Swim2s current run was scaled down using a = gallon bucket with ##% bo0esRIt 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.