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soluble, and is
crystallizable in this solvent to yield "beautiful, compact, clear, on sixsided
cut-crystal plates that melt with decomposition at 235-240° C."
This is obviously the way to go. The hydrazide should be
recrystallized from absolute ethanol, and then dried under a vacuum to
remove residual alcohol clinging to the crystals. About 300 ml of hot
ethanol is required to dissolve each gram of lysergic acid hydrazide
during the crystallization. Upon cooling, a first crop of pure lysergic
acid hydrazide is obtained. Then, by boiling away half of the mother
liquor and cooling, an additional crop is obtained. This process can be
continued as long as the crystals obtained look nice.
Practical LSD Manufacture
Step Two: Lysergic Acid
In this reaction, one mole of lysergic acid hydrazide is dissolved in
an inert, water-miscible solvent like ethanol. Then an excess of 1-molar
hydrochloric acid is added to form a salt with the lysergic acid
hydrazide. To this mixture is then added two moles of acetylacetone
(2,4-pentanedione), which forms the desired pyrazole. This reaction is
not nearly as touchy as the formation of the hydrazide. The presence of
traces of moisture from the air poses no problem. 2,4-pentanedione finds
use in analytical chemistry as a chelating agent for transition metals,
and as such should be available without raising too many red flags.
Synthesis of this compound is not hard, and directions for doing so are
found in US Patents 2,737,528 and 2,834,811.
To do the reaction, the flask containing the 5 grams of hydrazide is
wrapped in a single layer of foil to exclude light. Then a magnetic
stirring bar is added, along with 18 ml of ethanol, 18 ml water, 20 ml 1-
molar HC1 (made by adding one part 37% HC1 to 11 parts water) and
this mixture is stirred for a few minutes. Then 3.5 grams (3.5 ml) of
2,4-pentanedione is added at room temperature, and the stirring
continued for an hour or so.
The product is recovered from solution by the slow addition with
stirring of 20 ml 1-molar NaOH (40 grams per liter). This
neutralization throws the pyrazole out of solution as a solid. The solid is
collected by filtration through a Buchner funnel, and rinsed off with
LSD Directly From The Lysergic Amides —
The One Pot Shot 29
some water. The crystals are then dried under a vacuum, preferably
with the temperature elevated to 60° C. Further purification can be
done by crystallization. If so desired, dissolve the crystals in
chloroform, then add 8-10 volumes of ether to precipitate the product. I
do not feel this is necessary if the hydrazide used was reasonably
pure, since all the reagents used in the last step are soluble in water.
The water rinse should have carried them away. Further, alcohol and
2,4-pentanedione are volatile, and would be removed in the vacuum
This simple and easy reaction is done as follows: In a flask
wrapped in a single layer of foil