(Chief Bee)
01-08-04 12:38
No 481216
(Rated as: excellent)
4.3 Law Enforcement: An Interview With an LSD Clandestine Chemist
Richard Laing & John Hugel
Hallucinogens: A Forensic Drug Handbook, Chapter 4: Methods of Illicit Manufacture, p 182-183, Academic Press 2003.
Illicit LSD manufacturing has occurred since the early 1960s when the popularity of this drug was increasing as more young individuals discovered its psychedelic powers. At the epicenter of this "self discovery" movement stood a small group of individuals, some of whom preached the power of self-awareness, while others prepared the "psychedelic sacraments." It is worthy to note that few LSD clandestine laboratory seizures have been made since the earls to mid-1970s and it is presumed that the world's production of LSD is still controlled by a small group of individuals.
In September 1996 in suburban Vancouver, Canada, a Royal Canadian Mounted Police investigation culminated in the seizure of a clandestine laboratory. The significance of this seizure was unknown at the time. After extensive fingerprint database search, all of the seized identification and passport documents were either forgeries or of deceased individuals, the identity of the principal character was determined. (See Plate 4.6)
The chemist, an American fugitive, had jumped bail in 1974 after appealing a conviction for manufacturing LSD in California in 1973. He had been at large for more than 20 years and continued to ply his skill in the production of the "psychedelic sacraments." He granted a debriefing interview (Laing, 1999) just prior to his deportation to California. The chemist started cooking hallucinogens and LSD in 1962-63 using the Pinoche method - trifluoroacetic anhydride on lysergic acid. He discussed his role in the "League of Spiritual Discovery" in the preparation of the "sacraments" and as a guide for enlightenment (he perceived himself to still be in this role). Timothy Leary founded this group in the early 1960s. He discussed how another underground chemist taught hint how to make LSD using the DMF-SO3 complex which he said was a difficult reaction due to the toxic nature of sulfur trioxide and the critical stoichiometry of the reagents. In the 1996 seizure the chemicals and reagents for three different reactions were found: the phosphorus oxychloride reaction, CDI reaction and the DCC with HOBT reaction. When asked, he said that his main synthetic route used at the time was the CDI reaction since his diethylamine was in short supply. His preferred method, however, was the phosphorus oxychloride reaction, although it required too much diethylamine: 1 mol lysergic acid monohydrate to 2 mol POCl3 to 9 mol of diethylamine. He stated that the CDI method required the removal of the dimethylformamide solvent for which a two-stage vacuum stripping with a rotary evaporator, chiller and a dry ice condenser were needed. When asked about ergotamine, of which he and his co-conspirators had smuggled 24 kg into Canada, he said he would obtain 375g of lysergic acid monohydrate from 1 kg of ergotamine tartrate and that he only had 2 kg of ergotamine left but no lysergic acid. He would purchase ergotamine in kilogram lots for $3-$7 per gram, depending upon the source. The epimerization of iso-LSD was accomplished using his own method in which potassium metal is dissolved in anhydrous ether and then refluxed with anhydrous methanol. After returning to room temperature the iso-LSD was added to the potassium solution and allowed to sit 24 hours at room temperature in the dark, providing a "98.5%" conversion. He argued that the old standard method of refluxing in potassium or sodium hydroxide provided only yields of 75% or less. Purifying by means of recrystallization from methanol worked best and the purity was estimated by means of the "flash test" - the piezoilluminesence [sic] characteristic of pure LSD when two crystals were struck together. Seized at the lab were numerous drugs in varying quantities: LSD 47g, MDA 3 kg, MDMA 3 kg, MDEA 4kg, DMT 4 kg, diethyl- and dipropyl-tryptamine, 2C-B (4-bromo-2,5-dimethoxyphenethylamine), mescaline, trimethoxyamphetamine, dimethoxyamphetamine, psilocybin and numerous sets of standards.
Also found were 2g each of Iysergic acid sec-butylamide and iso-lysergic acid sec-butylamide. When asked about the "designer" LSD, he said that he did not base enough time to try it out and was not sure as to the dosage level. In the end he claimed to have made 900g of LSD that year.
The chemist said that his "first love" was dimethyltryptamine (DMT) and that he was synthesizing this compound before he started making LSD in the early 1960s. The DMT was made using a large 72 L reaction set-up and reacting indole with oxalyl chloride and then with anhydrous dimethylamine. The DMT required distillation and recrystallization to obtain pure product. Distillation would be set up on the laboratory lattice (Figure 4.6) and 1 or 2 kg would be processed at a time. A kilogram of DMT dissolved in 2L ether would recrystallize when added to 8L hexane. Rhomboid crystals would spontaneously form in the mother liquor.
Reference documents and hand written notes were found describing the use of monoamineoxidase (MAO) inhibitors, namely harmine and harmaline, with DMT to make it orally active. When asked about other tryptamines such as 5-methoxytryptamine he said he did not enjoy it but liked psilocybin. He went on to say that he did not care for the harshness of the hallucinogenic amphetamines (substituted phenylisopropylamines) but preferred the substituted phenethylamines such as 2C-B and mescaline which provided "enlightenment."
The interview ended with the chemist being escorted in to a waiting van for the trip to the airport and then on to California to serve the remainder of his original sentence.
The Hive - Clandestine Chemists Without Borders
(Stranger)
01-08-04 15:16
No 481258
The CDI method he describes - I take he is referring to Carbonyldiimidazole?
When he decribes evaporation of the DMF, this 2-stage vac. stripping with the chiller and dry ice condenser - is this for large quantities? I've seen small quantities of DMF evaporated without all this, just wondering what he was doing. In case one wanted to use larger quantities in the future.
(Chief Bee)
01-08-04 15:24
No 481263
The CDI method he describes - I take he is referring to Carbonyldiimidazole?
Yes.
When he decribes evaporation of the DMF, this 2-stage vac. stripping with the chiller and dry ice condenser - is this for large quantities?
If you do not use a cold trap together with such a strong pump, a lot of the DMF would end up in the pump oil, and you would have to change it frequently to maintain a high vacuum. It's your desicion which is the most cumbersome procedure.
The Hive - Clandestine Chemists Without Borders
(Hive Bee)
01-10-04 15:52
No 481674
on this guy and his techniques (i.e. is it worthwhile to get the book for knowledge)?? Also, did it state the source country of his kilograms of Ergotamine?
Love that isomerization technique he had with the metallic potassium, etc. (That 98.5% conversion rate is even better than the technique using tetrabutylammonium hydroxide, which gives 81% conversion rate.) Refluxing potassium metal in a flask full of ether and methanol - those solvents had better be anhydrous!
(Chief Bee)
01-10-04 18:19
No 481707
There's nothing more on that guy in there, but it's definitely a good book - Shulgin has also written a chapter on the pharmacology and structure-activity relationships of psychedelics.
The Hive - Clandestine Chemists Without Borders
(Newbee)
01-13-04 11:01
No 482219
great article thanks for posting! I'm assuming that's the nick sand bust, I read somewhere that his lab was literally better and more equipped than the health canada lab.
(Hive Bee)
01-27-04 13:32
No 484958
As for the KOMe method used...............its such a generic lab chemical that i cant believe it would be highly watched. Certainly someone working in a legitimate lab could order it without anyone blinking an eyelid.
Fan of Shulgin
Peace, love and empathy
02-09-04 05:37
(Rated as: UTF Google / check a book)
(Stranger)
04-22-04 16:50
No 502342
for using KOMe to epimerise iso-LSD could someone epimerise a whole lot of racemic LSD into LSD using this method (or any other)? 98.5% conversion would put 50% + and 50% - LSD to 'pretty freakin' close to 100% LSD would it not? then perform a flash chromatography over alumina with a 3:1 toluene:chloroform eluent and finally recrystalize with methanol... any problems with this?
(Hive Bee)
04-22-04 20:07
No 502390
The DMT required distillation and recrystallization to obtain pure product. Distillation would be set up on the laboratory lattice (Figure 4.6) and 1 or 2 kg would be processed at a time. A kilogram of DMT dissolved in 2L ether would recrystallize when added to 8L hexane. Rhomboid crystals would spontaneously form in the mother liquor.
Am I the only person who thinks the section i highlighted in bold is puzzling? why does it say that distillation was done in a laboratory lattice, big fuckin deal, so what if it was a lattice or a series of retort stands instead?
hmmm one good piece of info there though - i saw this quoted somewhere before, about the ether/hexane recrystallisation method - Would the same thing happen in DCM or other chlorinated solvent (since they're similar to ether in terms of their selectivity and high solvation power with these amines)? It would be nice to establish a simple and effective method of getting the dmt fb out of the nonpolar without evaporating it off or flash distilling (i want a method that requires no heat)... What is the solvents that dmt is most and least soluble in, preferably selected from a list of relatively OTC solvent sources (requiring nothing more than fractional distillation at the most to render usable) - ok here's my list: ligroin, n-hexane, dcm, tce, toluene, xylene, chloroform, ethyl acetate, acetone, mek... i'm sure there's more but i can't think of any just now.