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lt-up pressure from the flask. If the
stirring bar bangs too violently in the flask, remove it with a magnet
rather than break the flask.
Pour the contents of the flask into a 250 ml sep funnel, and drain
the lower layer (water solution of lysergic acid hydrazide tartarate)
into a 250 ml Erlenmeyer flask wrapped in foil. To the ether layer still in
the sep funnel, add 50 ml fresh decimolar tartaric-acid solution, and
Examine the water layer for the presence of lysergic acid hydrazide with a black light.
If there is a significant amount, add this also to the Erlenmeyer flask. Place the magnetic stirring bar in the Erlenmeyer flask, and stir it moderately. Monitor the pH of the solution with a properly calibrated pH meter, and slowly add .5M (20 grams per liter) sodium hydroxide solution until the pH has risen to the range of 8-8.
Higher pH will cause racemization. The freebase is then extracted from the water solution with chloroform. Two extractions with 100 ml of chloroform should complete the extraction, but check a third extraction with the black light to ensure that most all of the product lysergic acid hydrazide has been extracted. The chloroform extracts should be evaporated under a vacuum in a 500 ml flask to yield the product.
This is best done by rigging the 500 ml flask for simple distillation, and applying an aspirator vacuum to remove the chloroform. Assume that the yield from this procedure will be about 5 grams of lysergic acid hydrazide if ergot was the crop used. Assume that the yield will be about 7.5 grams if seeds were used. The difference here is due to the fact that in ergot, the amides 4 LSD Directly From The Lysergic Amides — The One Pot Shot 27 are largely composed of substances in which the portion lopped off is about as large as the lysergic acid molecule. Seeds tend to be more conservative as to their building upon the lysergic molecule. A careful weighing on a sensitive scale comparing the weight of the flask before and after would give a more exact number. Both of these choices are really very poor, because lysergic acid hydrazide, unlike most other lysergic compounds, crystallizes very well with negligible loss of product.
At the hydrazide stage of LSD manufacture, one has a perfect opportunity to get an exceedingly pure product, freed from clavine alkaloids and other garbage compounds carried in from the extraction of the complex plant material. I refer the reader to US patent 2,090,429 issued to Albert Hofmann and Arthur Stoll, the dynamic duo of lysergic chemistry, dealing with lysergic acid hydrazide. In this patent, they describe in a rather excited state how they were able to produce pure lysergic acid hydrazide from tank scrapings that were otherwise impure junk.
Lysergic acid hydrazide has the following properties: it dissolves easily in acid, but is very difficultly soluble in water, ether, benzene and chloroform. In hot absolute ethanol it is slightly