More Stuff.

How to
make LSD > So just _how_ does one make LSD ? HOW TO MAKE
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LSD : d-lysergic acid diethylamide
----------------------------------------------------------------------- OK This
file is about LSD . . I will detail some methods of making itfrom chemicals and from
seed. . It should be noted that this file is for informational purposesonly. . :) :)
HISTORY --------- LSD was first taken in its pure
form by D r. Albert Hoffman, a 37 year old Swiss chemist who worked at the Sandoz
Pharmaceutical labs inBasel. 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 deliberatlyswallowed some more, beginning
with the tiny dose of 250 micrograms,or 25 millionths of a gram, a dose so small
that no other drug knownproduces effects at these levels (200 micrograms is now
considered astandard dose of LSD ), and unbelivably to him he started trippingout. .
Sandoz did further tests and these confirmed the enormouspsychoactive 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 wellas testing it
for possible uses in reversing brainwashing ofsoldiers. . There were secret tests
done as well in which soldiers wereunknowingly dosed and observed, also many were
done in which they wereknowingly dosed, and the films of these disorientated
soldiers in awartime situation were shown to demonstrate the great potential for
LSD . Anyone outside the military can really only guess at the extent of testing
hidden from the public. The Russian scientists experimentedwith its warfare
potential as well as parapsychological uses ofLSD . The Weather Underground
alledgedly held acid sessions to see ifthey had been infiltrated by an informer.
The medica l profession alsolatched onto LSD , testing it for possible uses in
rehablilitatingpsychotics and schitsofrenics with some positive results. Similar
goodresults were recorded for people with heavy sex hang-ups, peopleaddicted to
drugs, and psychopaths. FORMS OF ACID
--------------- ACiD is normally sold in trips, little blotter paper tabs about
1cmbig although the size varies. . It can also be liquid, crystalline inpowder form
or in tablets of any description eg- microdots. . Thestandard dose is around 200
mics but the strength of the ACiD willvary enormously of course, as will the
quality of the high. Thediffent types of LSD eg (LSD -25, LSD -21, LSD mirror 21) all
givevastly different trips and each one is of course variable. I thinkthat the
crystalline and the liquid forms are the purest.
MAKING LSD ----- PT 1 - EXTRACTING
LYSERGIC ACID FROM SEED -------------------------------------------
First get your seeds of preferably W1oodrose (argyria [hawaiian babywoodrose])
variety but Convolvulaceae, Rivea, or Ipomoea will do. . Theoverall yield with this
method is low, however it can be done witheasily obtained chemicals. . NOTE - the
following procedure requiressome knowledge of lab techniques and unless you know
what you aredoing you could easily blow yourself up, or poison you and yourfriends
if the final product is imperfect. . Proceed with caution. .
--- Finely grind seeds and add NaHCO3. Extract with ethyl acetate bysoaking about
one day. Filter and extract the ethyl acetate withtartaric acid solution. Basify
the extract with NaHCO3 and extractwith ethyl acetate. D ry and evaporate the ethyl
acetate to get thealkaloids. Repeat this procedure on the seeds until no more
residue isobtained. This residue contains the natural alkaloids which aresimilar to
LSD , as well as other plant products and impurities. Add 100ml petroleum ether to
100g finely ground seeds and let soakabout two days. Filter, discard and let seeds
dry. Add 100 ml methanolto the seeds let soak about two days. Filter, repeat
extraction withanother 100ml methanol and evaporate the methanol extracts invacuum.
This yellow residual oil contains the alkaloids. ERGOT
ALKALOID HYD ROLYSIS --------------------------- NOTE about
ergot. In order to make LSD , lysergic acid isneeded. This can sometimes be
obtained, but generally one of thelysergic acid containing ergot alkaloids such as
ergotamine is morereadily available. Ergot is the dried sclerotium of various s
peciesof fungi which infect rye (and other grasses) leading to the formationof
large purple growths in place of the rye grains. These growths are
collected,dried,powdered and the alkaloids extracted. Ergot is mainlyproduced in
Europe (especially Switze rland). Some is grown in theUSA, mainly for the use of
ergotamine and related compounds inmedicine (terminating migrane headaches etc)
Many of the ergotalkaloids are deriatives (amides) of lysergic acid. Unfortunatly
thesecompounds have little halluci nogenic activity and it is necessary tohydrolyze
(split with water) off the amide, producing lysergic acidand to synthesise a
different amide with greater psychadelicactivity. This hydrolysis can be done with
any of the following compounds 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 inactiveiso-LSD . A conversion process is
detailed below. D issolve 20mg of the alkaloid (previous extraction) in 200ml 1M
KOHin methanol (ie. dissolve 56g KOH pellets in 1L 100% methanol) in a 1Lheavy
walled vacuum flask and evaporate the methanol in vacuum at roomtemperature. To
prevent flask from cooling, thus prolonging theevaporation time place flask in a
pan of water maintained at roomtemperature by gently heating or warm water running
through. Add 400ml 8% KOH in water to the residue and boil for one hour (under N2
ifpossible-this can be done by filling the flask with an N2 stream andloosely
stoppering or by allowing a gently stream of N2 to flowthrough during heating.
Cool, acidify with dilute sulfuric acid andshake in separatory funnel with 1L
ether. D iscard the upper etherlayer and filter the aqueous suspension of lysergic
acid(I) invacuum. Wash precipitate with 20ml dilute sulfuric acid. To recoverthe
small amount of (I) in solution remaining in solution, basify theNa carbonate and
bubble CO2 through it. Filter and add precipitate tofirst batch. Some isolysergic
acid will remain in solution and can beprecipitated by adding 10% HNO3. It can be
converted to (I) by adding3ml 10% KOH for each 0. 1g acid, boiling on steam bath for
one hourunder N2(if possible) and precipitating by acidifying with glacialacetic
acid. Maximum yield is about 9g (I) for 20gergotamine(alkaloid).
PURIFYING ----------- About 20% of (I) will be
isolysergic acid(non psychoactive) and itcan be isomerized to (I) by the above
procedure. Purifying is not nessecary but can be done to improve quality as
follows. . D issolve 9g (I) in 20ml NH4 OH, filter and concentrate in vacuum atroom
temperature to precipitate (I). After filtering, the greycrystals can be further
purified by dissolving in boiling water andcooling in ice bath to precipitate (I).
Melting point (point itdecomposes at) is about 240�C Alternatively the dark
coloured (I) resulting from hydrolysis can beshaken with 2 X 400ml 2 M NH4 OH in
ethanol and the combined extractsevaporated in vacuum to give (I). D issolve the
remaining residue in500 ml hot methanol, cool to 0�C and filter out the (I).
Coloured impurities can be removed by shaking solution withdecolourizing carbon and
filtering. MAKING LSD
------------ LSD FROM LYSERGIC ASID
------------------------ D issolve 13. 4g dry (I) in 250 ml dry dimethformamide and
cool to0�C. Add cooled solution of 3. 4 ml 0. 35 M methanesulfonic acidanhydride in
dry dimethylformamide. After thirty minutes at 0�C add14. 6g (20. 4 ml) diethylamine
(D EA) and keep at 0�C for o nehour. Evaporate in vacuum to get LSD . D issolve 5. 3g
dry (I) in 125 ml acentonitrile (or dimethylformamideor proprionitrile) and cool to
-20�C (freezer or dry ice-acetone orethanol mixture). Add 8. 82g trifluroacetic
anhydride in 7 5 mlacetonitrile cooled to -20�C carefully. Let stand at - 20 for 1*
hoursor until all (I) dissolves. Then add 7 . 6g D EA in 150ml acetonitrileand let
stand at room temperature in dark two hours. Evaporate invacuum to get LSD .
D issolve 0. 536g (I) in 10 ml freshly distilled POCL3; stir and add416mg powdered,
freshly sublimed PCl5. Hold two minutes at roomtemperature, two minutes at 90�C,
and evaporate in vacuum. Extract theresidue with hexane to give the
lysergic acid chlo ride-HCl (can alsoextract the reaction mixture with hexane
instead of evaporating invacuum). Alternatively use 6ml POCl3 and 240 mg SOCl2 and
heat threeminutes at 90�C to get the acid chloride. To 5g of the acid chlorideadd
1. 4ml D EA in 50ml methane c hloride and cool to 0�C. Stir and add27 . 5 ml pyridine
and stir * hour at 0� . Warm to room temperature andstir 1* hours. Evaporate in
vacuum to get LSD . To a suspension of 13. 4g dry (I) in 800ml dry
dimethylformamide(D MF) in a 2L vacuum flask at 20�, add a solution of 8. 9gN,N'-
carbonyldiimidazole in 250ml D MF and stir at 20� in dark for *hour. Add a solution
of 4g D EA in 50ml D MF and let stand 2 hou rs at20�;then purify or dissolve residue
in 2*L 2% tartaric acid; NH4OH andextract with a 9:1 solution of ether:ethanol. D ry
and evaporate invacuum to get LSD . Add 1L dimethylformamide (freshly distilled if
possible) to dryflask fitted with stirrer, ice bath, dropping funnel and condenser,
both protected from water by Ca chloride drying tubes. Add dropwisewith stirring
over 4-5 hours at 0� 0. 21bs (90. 7 g) So 3 (sulfuricanhydride, available as Sulfan
from Allied Chem Co. ) if precipitateforms, stir until it dissolves. Sulfan may be
made in larger amountsand is good for several months if kept dry and cool. Molarity
of freshSO3-D MF reagant should be about 1M, but for precise determination adda
little water to aliquot and titrate with standard NaOH tophenolphthalein end point.
Add 6. 45g dry (I) (or 7 . 15g (I)monohydrate) and 1. 06 LiOH hydrate to 200ml
methanolin a 1L vacuumflask and evaporate in vacuum. D is olve residue in 400ml D MF
at about15mm Hg through a twelve inch column packed with glass helices orother
material. Cool to 0� and rapidly add 50ml SO3-D MF solution (1M). Stir at 0� for ten
minutes and add 91. 5g (12. 9ml) D EA and stir tenminutes. Add 400ml water, stir and
add 200ml saturated NaCl. Extractthe LSD by shaking with several 500ml portions
ethylene dichloride(can use indole test to show completeness of extraction).
Combineextracts (lower layor in seporatory funnel) and dry, evaporate invacuum to
get LSD . To a reflexing slurry of 3. 15g dry (I)(or monohydrate) in 150mlCHCl3 add
0. 1 mole of the amine in 25ml CHCl3 and 2ml POCl3simultaneously from seperate
dropping funnels over 2 to 3minutes. Reflux 3 to 5 minutes more till a clear amber
solution results. Cool to room temperature and wash with 200ml 1m NH4OH. D ry and
evaporate in vacuum(below 40�C). Can dissolve in the minumum amount ofmethanol.
Filter and wash crystals with cold methanol and acidify witha fresh solution of 20%
maleic acid in methanol . Filter and washcrystals with cold methanol to get the LSD
or other amide. This methodworks with a wide variety of amines. For LSD itself, the
POCl3 can beadded first. The yield is about 50%.
PURIFYING ----------- To purify your extracted LSD
dissolve the residue in 150ml CHCl3and add 20ml ice water. Pour into *L seperatory
funnel and drain outthe lower CHCl3 layer into a beaker (after shaking). Add 50ml
CHCl3 tofunnel, shake and drain bottom layer into same beaker. Repeat with 3 X50ml
CHCl3 and discard the water. Extract the combined CHCl3 extractswith 4 X 50ml ice
cold water and dry, evaporate in vacuum the CHCl3 toget 3. 5g d-LSD . This is
composed partly of inactive d-iso-LSD whichcan be recovered and c onverted to d-LSD
as follows: dissolve theresidue in 120ml benzene and 40ml CHCl3 (or 200ml
methanol), addtartaric or maleic acid and shake to precipitate mainly d-LSD (add a
little ether and cool in refrigerator several days if nessecary toensure comp lete
precipitation)) Evaporate in vacuum the solvent toget d-iso-LSD . Ad 50ml ethanol
and 5ml 4N KOH per g iso-LSD and letstand at room temperature for two hours,
evaporate in vacuum (orextract with CHCl3 as above) to get LSD .
SYNTHESING LSD ---------------- Another way to go about
it is to synthesise LSD entirely as I willnow detail. SYNTHESIS OF
2,3-D ihydrolysergic acid -----------------------------------
Condense methyl-6-methyl-nicotinate and 5-Br-isatin by fusion at180� to get 57 %
yield of (I) (I) in boiling glacial acetic acid istreated portionwise with powdered
zinc and refluxed one hour to get(II). Treat (II) with NaBH4-BF3 (in ether) in
tetrah ydrofuran asabove to give (III) which when treated 24 hours with acetic
anhydridegives (IV). Treat (IV) with methyl iodide in methanol-acetone in aCarius
tube to get (V) which is reduced with KGH4 in aqueous methanolto get (VI). Treat
(VI) with NH3 co ntaining NaNH2 for one hour to get2,3-dihydrolysergic acid (VII)
which can be converted to2,3-dihydro-LSD which is about ten times less active than
LSD . (VII)can be converted to lysergic acid prior to conversion to LSD , whichwill
triple the yield in t erms of LSD activity. D ehydrogenation may work for the next
process and also may work forconverting 2,3-dihydro-LSD into LSD .
LYSERGIC ACID FROM 2,3-D ihydrolysergic acid
------------------------------------------- To synthesise Lysergic acid from 2,3-
dihydrolysergic acid dissolve4g (VII) in 7 8ml 1. 5% KOH and reflux five minutes
(under N2 ifpossible). 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. 6with HCl; filter and wash
precipitate with water to get 1g lysergicacid. 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 onehour at 90�. Add 20ml water
and evaporate in vacuum. ( Purify byadding ether and aqueous tartaric acid, basify
the aqueous phase andextract 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 HCladd with good stirring
at 0W 4ml 1N Na nitrite. Quickly over 2-3minutes add 40ml 0. 1 N NaHCO3 and extract
with 100ml ether, then 50mlether. Wash ether with water and dry and evaporate in
vacuum at10�. D issolve the resulting yellow azide in about 5ml diethylamine(D EA)at
0� and heat one hour at 60� in a bomb(sealed metal pipe). Let standseveral hours
and ev aporate in vacuum to get about 0. 7 g d-LSD and0. 15g d-iso-LSD (convert as
above). Alternativly the D EA can be addedto the cooled ether solution of the azide
and let stand several hoursor overnight at room temperature in the dark in a vented
flask. LSD ID ENTIFICATION
------------------ There are a few ways to test for LSD presence and strength. .
LSD fluoresces under an ultraviolet light (black light), but so domany other
compounds. As LSD is an indole deriative it shows positive to these indoletests
(which will also show D MT, psilocybe etc. ) KELLER TEST Add a little of the
powdered substance (0. 2mg) to 1ml glacial aceticacid containing 0. 5% FeCl3; layer
underneath with 1ml concentratedsulfuric acid and shake. The colour varies with the
indole. (Olivegreen - psilocin ; Red-Violet - psilocybin) VAN URK TEST Prepare
Van Urk reagent by adding 0. 5 g p-dimethylaminobenzaldehyde,100ml water, 100ml
concentrated sulfuric acid. D issolve 1mg substanecin 1ml ethanol and mix with 2ml
Van Urk reagent and illuminate for 10minutes 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 severalmonths. Put a
little of the suspect substance in a few drops ofethanol (gin may do as a control),
wet a filter paper strip in thisand 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 orviolet blue
indicates indole deriatives such as LSD . With D MT orpsilocybin the colout is
redder. The colour must be observed soonafter adding the HCl as it rapidly changes.
COMPLETE SYNTHESIS OF LSD --------------------------- Mix
32. 8g (0. 217 M) methyl-6-methylnicotinate (other alkyl groupscan 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 flaskat 100� in an oil bath and raise the temperature to
1 7 0� and letreact for 7 0 mins. Cool and then grind the solid as fine as possiblein
a mortar. Recrystallize from 150ml dimethylformamide and wash withether 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 smallportions over 30 mins excess
powdered zinc. Reflux one hour, filterand evaporate in vacuum and recrystallize the
residue from dioxane toget 9. 7 g(95%) methyl(5-bromo-2-oxindol-3-yl)-6-
methylnicotinate (II)to get a suspension of 18g dry NaBH4 in 300ml dry
tetrahydrofuran addwith stirring at 0� over 30 mins about 7 5g BF3 etherate. Stir 3
hoursat 0�, add 18g (II) and heat exactly 20 mins at precisely 22-24�. Addcarefully
150ml concentrated HCl while cooling. Add 200ml water andstir 12 hours. Basify,
extract the product with ethyl acetate anddry,evaporate in vacuum to get 11g of
residue which recrystallizesfrom 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 aceticanhydride then
hydrolyze and extract to get 11. 5g residue which isground in petroleum ether and
recrystallized from cyclohexane (canchromatograph on alumina and elute with
petroleum ether t o was out anoil, then with benzene containing 5% ethyl acetate to
elute theproduct) to givemethyl-(1-acetyl-2,3-dihydro-3-indolyl)-6-methylnicotinate
(IV). Heat5g (IV), 12. 5ml acetone, 12. 5ml methanol and 1. 8ml methyl iodide for18
hours in a Carius t ube at 7 0�-80� C. Cool, filter, wash withacetone and
recrystallize from methanol to getmethyl-(1-acetyl-2,3-dihydro-5-bromo-3-indolyl)-
1,6-dimethylnicotinateiodide (V). To 9. 4g (V) in 250ml water and 250ml methanol at
35� addover 5 mins 2. 9g KBH4 and stir 10 mins. Add 2. 9g more KBH4 and stir 30mins.
Evaporate in vacuum and extract the residue with methylenechloride to get about
6. 2g oily mixture containing about 2g of the disomer (can seperate by
chromatography if desired) ofmethyl-(1-acetyl-2,3-dihydro-5-bromo-3-indolyl)-6-
methyl-1,2,5,6-tetrahydronicot-inate(VI) To a suspension of finely powdered NaNH2
(6. 1g) in 2 litres dryammonia, add with stirring 8g (VI) in 50ml dry
tetrahydrofuran. Stirone hour, add NH4Cl and evaporate the ammonia as fast as
possible in anitrogen stream. Extract at pH 8 with methylene chloride to get 6g(can
chromatograph on 300g silica gel and 250g celite and elute with98% benzene-2%
absolute ethanol and evaporate in vacuum) ormethyl-1-acetyl-2,3-dihydro-lysergate
(VII) One method of dehydrating (VII) is above under LYSERGiC ACiD FROM2,3-
dihydrolysergic acid and another follows. Warm to dissolve 1. 5g 2,3-dihydro-LSD
in 5ml acetone, 40ml waterand 40ml saturated NaHCO3. Cool to 20� and add all at
once withvigourous stirring 2. 46g potassium nitrosodisulfonate dissolved in90ml
water and 10ml saturates NaHCO3. After 1 min, extra ct 7 timeswith ethylacetate,
wash the combined extracts with water, dry andcarefully remove solvent to get a
mixture of 12-OH-LSD , LSD andstarting material which can be chromatographed to give
about 0. 2g12-OH-LSD . The following method of converting (IV) to the diethylamide
(whichcan probably be used in place of (IV) to give the diethylamide of (V),(VI)
and (VII)) will probably also work admirably for (VII) orlysergic acid. Reflux
0. 5g (IV) with 0. 5 KOH in 30 ml methanol for 4hours. Evaporate in vacuum and add
water to the residue. Adjust the pHto between 5 and 6 and filter or centrifuge to
get 0. 3g of the freeacid. Suspend 1. 8g of the acid in 125ml chloroform, cool to
minus 5�and add 0. 5g triethylamine, then 0. 6g ethylchloroformate and stir 45mins.
Add 2 ml diethylamine and stir 3 hours at room temperature toget, after the usual
workup 1g of the diethylamide (recrystallize frombenzene)
dOCs tYPEd bY ShR�Ud
On tHe 13TH oF JUlY
1993