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strong ammonia (28% NH3), 350 ml distilled water, 190 ml 10%
gelatine solution, and 700 ml 12.5% bleach. This strength of bleach is
Practical LSD Manufacture
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available from pool supply companies and makers of cleaners. The
5.25% strength Clorox will not do here. One must also be aware that
traces of iron and copper have a very bad effect upon the yield, so do
not dispense with the use of distilled water. The bleach is another
possible source of iron. In checking out this reaction, the Pro
Chemicals brand of bleach worked fine. I can't vouch for other
brands. If all else fails, the bleach can be made from chlorine and
NaOH in distilled water. (See Organic Syntheses Collective Volume 1,
page 309.) The Pro Chemicals brand of bleach analyzed at 10 ppm iron
by atomic absorption, and this amount did not interfere with the
reaction. One must also check the bleach to make sure it is alkaline, as
free chlorine prevents the formation of hydrazine.
When the ingredients have been mixed in the baking dish, it is
heated as rapidly as possible until it has been boiled down to one-third of
its original volume. Being a wimp and boiling it down too slowly
reduces the yield. Take not more than two hours.
The dish is then removed from the heat, and allowed to cool.
When the dish nears room temperature, it should be nestled in ice to
chill thoroughly. The solution should then be filtered to remove
suspended particles from the solution.
The filtered solution is next put in a beaker, and nestled in ice
mixed with salt until the temperature of the solution reaches 0° C.
When that temperature is reached, 10 ml of concentrated sulfuric acid
for each 100 ml of solution is slowly added with constant stirring. If
the stirring is not strong, or if the filtering was poorly done, a product
contaminated with brown particles results. If done well, hydrazine
sulfate precipitates as white crystals. The mixture is allowed to stand in
the cold for a few hours to complete the precipitation. The crystals are
then filtered by suction, and the crystals rinsed off with cold
alcohol. The yield is 25 to 30 grams of hydrazine sulfate.
4
LSD Directly From The Lysergic Amides
The One Pot Shot 35
Step Two:
Hydrazine Hydrate
Mix 100 grams dry hydrazine sulfate with 100 grams powdered
KOH and place the mixture into a copper and silver retort. Then add 15
ml water, and distill off the hydrazine hydrate formed though a
downward-inclined glass condenser. There is little need for heat to be
applied at the beginning of the distillation because so much heat is
generated in the reaction between the KOH and the sulfate. Later,
strong heating is required to distill out the last of the hydrazine
hydrate.
This crude product contains water beyond the monohydration of
hydrazine. It is purified by fractional distillation. Pure hydrazine
hydrate boils at 117° C to 119° C. The forerun contains the excess
water. It should be converted back to hydrazine sulfate by addition of
sulfuric acid as done in step one. The yield is 10 grams of hydrazine
hydrate.
During the fractional distillation, there are some precautions
which should be followed. Hydrazine hydrate attacks rubber and cork,
so the use of these materials must be avoided in the distillation. It also
attacks most kinds of stopcock grease. The distillation is most safely
done under nitrogen. Nitrogen should be introduced into the distilling
flask, and the system flushed of air for about 15 minutes. Then the
rate of nitrogen flow is reduced, and distillation commenced. The
product will also attack glass, albeit slowly. It should be stored in 304 or
347 stainless steel. 316 stainless is not acceptable.
Step Three:
Anhydrous Hydrazine
100 grams (100 ml) of hydrazine hydrate is mixed with 140 grams
powdered sodium hydroxide. The apparatus is thoroughly flushed
with nitrogen, then the rate of nitrogen addition to the distilling flask
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is slowed, and fractional distillation is commenced through an
efficient fractionating column of about 15 theoretical plates.
Anhydrous hydrazine distills at 112° C to 114° C. Anhydrous
hydrazine is obtained at 99%+ purity.
Another method for producing anhydrous hydrazine exists which
gives a higher yield of product, but it uses anhydrous ammonia and
more complicated glassware and procedures. See Journal of the
American Chemical Society Volume 73, page 1619 (1951), and
Volume 76, page 3914 (1954). Also see Hydrazine by C.C. Clark, The
Chemistry of Hydrazine by L.F. Audrieth, and Industrial and
Engineering Chemistry Volume 45, pages 2608 and 2612 (1953).
Also see Inorganic Syntheses Volume 1, page 90 (1939).
Anhydrous hydrazine can be stored in dark glass bottles under
refrigeration for years.
Other variations on the alkali hydroxide dehydration of hydrazine
hydrate exist which give higher yields of less-pure hydrazine. See
pages 48-54 in the Chemistry of Hydrazine mentioned above. It lists
many references. Especially interesting is Journal of the American
Chemical Society Volume 71, pages 1644-47 (1949).
Preparation of Diethvlamine
NH3 + CH3CH2I s> xHI + CH3CH2NH2
+ (CH3CH2)2NH +
(CH3CH2)3N
The reaction which produces diethylamine also yields as by-
products ethylamine and triethylamine. The relative amounts of each
compound produced depends upon the molar ratio of the two starting
materials. Use of only a little ethyl iodide favors the formation of
mostly ethylamine. Use of a lot of the ethyl iodide favors the
formation of triethylamine. Somewhere in the middle, a roughly even
split occurs. This will be done here. See Journal of the American
Chemical Society Volume 69, pages 836 to 838 (1947).
4
LSD Directly From The Lysergic Amides
The One Pot Shot 37
A section of clean steel pipe 2l/2 to 3 inches in diameter is
obtained, and fine threads are cut into each end so that a cap may be
screwed onto each end. A really nice touch would be to have all the
pieces plated with a half-thousandths-inch of electroless nickel, but
the plater may think you are constructing a pipe bomb when he sees
the pipe and caps.
The bottom of the pipe is secured by screwing the cap on over
threads coated with Teflon tape. Welding may also be used. The pipe is
then nestled into a Styrofoam cooler, and is then filled about Vi full of
rubbing alcohol, and then to this solvent dry ice is added, slowly at first
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