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the alumina, two zones that fluoresce blue can be spotted by
illumination with a black light. The faster-moving zone contains LSD,
while the slower-moving zone is iso-LSD.
When the zone containing LSD reaches the spigot of the burette, it
should be collected in a separate flask. About 3000 ml of the 3-1
benzene-chloroform is required to get the LSD moved down the
chromatography column, and finally eluted.
The iso-LSD is then flushed from the column by switching the
solvent being fed into the top of the column to chloroform. This
material is collected in a separate flask, and the solvent removed
under a vacuum. The residue is iso-LSD, and should be stored in the
freezer until conversion to LSD is undertaken. Directions for this are
also given in this chapter.
For the fraction containing the LSD, conversion to LSD tartrate
must be done to make it water soluble, improve its keeping
characteristics, and to allow crystallization. Tartaric acid has the
ability to react with two molecules of LSD. Use, then, of a 50% excess of
tartaric acid dictates the use of about 1 gram of tartaric acid to 3
grams of LSD. The three grams of LSD would be expected from a
well-done batch out of a total 3.5 LSD/iso-LSD mix.
The crystalline tartrate is made by dissolving one gram of tartaric
acid in a few mis of methanol, and adding this acid solution to the
benzene-chloroform elute from the chromatography column.
Evaporation of the solvent to a low volume under a vacuum gives
crystalline LSD tartrate. Crystals are often difficult to obtain. Instead,
an oil may result due to the presence of impurities. This is not cause
for alarm; the oil is still likely 90%+ pure. It should be bottled up in
dark glass, preferably under a nitrogen atmosphere, and kept in a
freezer until moved.
If chromatography reveals that one's chosen cooking method
produces little of the iso products, then the production of the tartrate
salt and crystallization is simplified. The residue obtained at the end
Practical LSD Manufacture
of the batch is dissolved in a minimum amount of methanol. To this is
then added tartaric acid. The same amount is added as above: one gram
tartaric acid to three grams LSD. Next, ether is slowly added with
vigorous stirring until a precipitate begins to form. The stoppered flask is
then put in the freezer overnight to complete the precipitation. After
filtering or centrifuging to isolate the product, it is transferred to a dark
bottle, preferably under nitrogen, and kept in the freezer until moved.
LSD from (so-LSD
Two variations on this procedure will be presented here. The first is
the method of Smith and Timmis from The Journal of the
Chemistry Society Volume 139, H pages 1168-1169 (1936). The other is
found in US patent 2,736,728. Both use the action of a strong
hydroxide solution to convert iso material into a mixture that contains
active and iso material. At equilibrium, the mixture contains about 2/3
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@Wednesday, December 19, 2018 4:36:45 PM