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Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

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 #1 
Old 2001-08-24, 06:39
madchemist madchemist is offline
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Default LSD, not so hard......

I have been looking at many LSD synths lately. People including myself used to say that making LSD was too hard for the average clandestined kitchen chemist. Now I'm not so sure anymore. That is a good thing
Here we will look at three ways, all starting from LSA.

Chloride route:
LSA + POCl3 (phosphorus oxychloride) or PCl5 (phosphorus pentachloride)--->lysergic acid chloride hydrochloride + diethylamine -->LSD.

This is one of the best synthesises. POCl3 is best to use, but PCl5 can be substituted, and is easily made from white phosphoruse (yes the kind in a florescent tube, I'll have to find the reference).
Basically, the LSA is dissolved in dry chloroform. A separate solution of diethylamine in chloroform is made and dryed. The two are mixed and brought to a slow boil for a few minutes. Then heat is removed and POCl3 or PCl5 (or both) is added at such a rate to keep the solution boiling for a few more minutes. Then the solution is boild slowly with external heat until an amber colored solution results. Then it is cooled, comcentrated by removing some solvent under a vacuum, and extracted with a tartaric acid + water solution, which is basified with sodium carbonate and extracted with ether. The ether is washed and dried, and stripped under vacuum. The residue left is chromatogrphed for purity, and then the LSD is crystallized with tartaric or maleic acid.

Another synth is the one I have up at chemhead. It is the azide route. Forming the azide of LSA and then condensing it with diethylamine.
LSA + hydrazine-->lysergic acid hydrazide
LSA-hydrazide + NaNO2-->lysergic acid azide
LSA azide + diethylamine-->LSD
Basically, LSA is refluxed with hydrazine under inert conditions (N2), then water is added and the solution boiled a little longer. This is cooled in the fridge and LSA-hydrazide precipitates. That is dissolved into conc. HCl, and so is sodium nitrite in a separate solution, both brought down to around -10 - -20 deg C. Then they are mixed, and pH is kept stable by adding more HCl acid. When pH is stable, the solution is basified with sodium carbonate and extracted with ether. The ether is washed and dryed, then stripped under a vacuum to yeild LSA-azide. The azide is then dissolved in methanol, and diethylamine is added. It is allowed to sit for about 24 hours, in which LSD and iso-LSD (the isomer being easily converted) forms. The methanol stripped off, and the result chromatographed and crystalized.

Next, and I like this one, is the ester route. It forms an ester of LSA using an alcohol and most organic and non-organic acids (the most popular non-organic being HCl). The ester formed will be correlated to whatever alcohol you use (i.e. butyl alcohol forms butyl ester, ethyl forms ethyl, methyl forms methyl, etc).
LSA + methanol(or whatever) + HCl-->Lysergic acid methyl (or whatever alcohol you used) ester
LSA-methyl ester + diethylamine-->LSD
Or posibly in a higher yeileding synth
trimethylaluminum + diethylamine--> trimethylaluminum diethylamide
TMA diethylamide + LSA-methyl ester-->LSD
LSA would be dissolved in dry methanol, cooled to about 0 deg C, and gassed with dry HCl gas till pH reached 0-1. This is allowed to stir gradually warming up to room temp overnight. Afterwards, the solution is either crystallized in HCl form by cooling solution on an ice-bath and adding ethyl acetate to obtain LSA-methyl ester HCl. Or by stripping off methanol, taking up residue in water, basifying with sodium carbonate, extracting with ether and stripping off ether to obtain LSA-methyl ester which could be used equally as well.
The ester can either be dissolved in DCM with diethylamine and heated to 40 deg C for a couple hours, or in the higher yeilding one, DCM diethylamine and trimethylaluminum can all be mixed first, then the LSA ester added and heating to 40 deg C. Both reactions are cleaned up by stripping off half volume under vscuum, extracting with tartaric acid and water solution, basify that with sodium carb and extract with ether. The ether is washed and dried and stripped off under a vacuum. The resdiue is chromatographed and crystallize.

Alright, thats it for now. Go ahead and ask questions, cause I know some of you will. There will be more, but I am still researching.
 #2 
Old 2001-08-24, 06:52
slpwlkr333 slpwlkr333 is offline
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Default Re: LSD, not so hard......

hydrazine and the government
 #3 
Old 2001-08-24, 09:19
madchemist madchemist is offline
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Default Re: LSD, not so hard......

How about this:
calcium hypochlorate + ammonia + gelatin--> hydrazine sulfate[62]
hydrazine sulfate + NaOH-->hydrazine[61]

I included the references.

[61] Brauer, Handbook of Preparative Inorganic Chemistry, p 469
[62] Adams and Brown, Hydrazine Sulfate, Organic Syntheses Collective Volume I, p 309,

 #4 
Old 2001-08-30, 18:21
bbell bbell is offline
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Default Re: LSD, not so hard......

Lsd is the hardest drug to manufacture. Inert atmospheres and done in darkroom are all necessary. Hydrazine when heated in the presence of air explodes. di-para-toluyl-l-tartrate must be used to obtain dextrorotary lysergic acid. Obtaining lysergic acid as it needs a D.E.A. licence. Do not believe a word of what you read on the net about any drug synthesis. This includes books published by 'Loompanics' & 'the anrachrist cookbook'Believe only chemistry journals
 #5 
Old 2001-08-30, 18:50
acidmelt acidmelt is offline
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Default Re: LSD, not so hard......

Not all sites post bullshit by Anarchist cookbook or other crap like that. I have many synths on my site that i can garuntee are acurate.

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CHEMHEAD CHEMISTRY
http://www.angelfire.com/mi3/chemhead
 #6 
Old 2001-08-30, 19:24
madchemist madchemist is offline
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Default Re: LSD, not so hard......

That POCl3 route is a widely accepted route.
Also that hydrazide-azide route is the route on ALbert Hoffmanns Sandoz Lab patent, and he did it using crude "ergotoxines" as he would put it. So you cant tell me it wont work.
As for chirality, KOH (or maybe even other bases) perform a good function for isomerization.
Nitrogen gas for inert atmospheres is obtainable, if you even use that route.
Darkroom conditions hard? No harder than screewing a 20watt red light into your lab socket.
LSA can be obtained through a few natural sources as well (like seeds, ergot, certain species of the clitocybe genus of fungi contain LSA and other ergot akaloids).

I dont beleive any synth I read in "Loompanics" books or whatever (which I dont even own any, all my info comes from the net). But I DO beleive the ones that are published in scientific journals, and US patents.
 #7 
Old 2001-09-01, 03:07
bbell bbell is offline
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Default Re: LSD, not so hard......

If people post their references with your synthesis it would be very helpfull.The U.S. patent office will send you a full article for $1. LSD patent no.'s are.2,736,728.,2,774,763 & 3,141,887 this is the lysergic acid and phosgene-dimethylformamide route.There is for you Japanese speaking people a route by Urakubo,Goro et.al.,in Eisei Shikenjo Hokoku vol88,pages 72-4 (1970)in Japanese. I also have several other routes from chemical journals. Most articles on the net fail to mention that lysergic acid must be resolved into it's dextrorotary configuration.I have done LSD in the 1960's and 70's.On the black market since then I have not run into LSD that can compare at all. What the chemists are doing wrong I do not know? But I have a lot of different synthesis the real synthesis.

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 #8 
Old 2001-09-01, 08:59
Mega-Volt Mega-Volt is offline
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Default Re: LSD, not so hard......

Wow,

acidmelt, you have an awsome chem page!
Unfortunatly I am completely Chem-dumb.
I am a huge LSD fan.
Can you recomend any chem books?
I would cut off my left thumb, to learn how to synth LSD. Not that I need any, but I think the WORLD needs more acid.




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You ate all of that?
 #9 
Old 2001-09-02, 06:07
nihilistic nihilistic is offline
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Default Re: LSD, not so hard......

i read and heard some where maybe from rhodium.ws that there is an easier way with lye bread and a fluro tube, you grow the stuff (fungus) in darkness then go from there

maybe not as easy as this

not sure.
 #10 
Old 2001-09-05, 03:27
madchemist madchemist is offline
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Default Re: LSD, not so hard......

The first two can be found with references at rhodium.ws/chemistry
The azide route was taken from patent num.
2438259, looked up at http://www.geocities.com/dritte123/PSPF.html.

Also, the use of a PCR to couple LSA and diethylamine may be the future. You would just dissolve lSA, diethylamine, and a PCR in a solvent, allow them to react for 15-30 minutes, and BAM LSD. PCR's are EXPENSIVE though, not too expensive, but expensive to the point as if you were synthesizing your own for profit, it would significantly close the profit margin. You want that to be as wide as possible.
 
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