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sulfuric acid in it.
figure 2 '— On
tne other side
of the adapter, a 2000
ml flask can be attached
containing 1000 ml of
acetonitrile or dimethylformamide. The use of stopcock grease
should be avoided, as SOs will attack it. Rather the joints should be
sealed by wrapping parafilm around them.
There will be a tendency for the two solutions to come into a
vapor equilibrium. 30% oleum contains about 580 grams per liter
SOa. The vapors will over time work their way into the solvent and
form complexes. It will take some time, depending upon the
temperature, for enough fumes from the sulfuric acid to work their
way out of the acid and into the solvent. Slow magnetic stirring in the
solvent helps to maintain a homogenous mixture, and speeds
absorption of SOa fumes. Cooling the solvent in ice can't hurt either.
Analysis of the solvent should be done after about 12 hours have
passed. The need for stirring is especially crucial here so a
representative sample is taken. To analyze, remove exactly 2 ml of
solvent with a pipette and squirt it into 50 ml of distilled water. Add
some phenolphthalein indicator, or monitor pH with a meter. Now
titrate with .IN NaOH (prepared by dissolving exactly 4 grams of
NaOH pellets in one liter of water) until the color of the solution turns
Adapter used in preparing SOj-solvent complex
from fuming sulfuric acid.
6 LSD From Lysergic Acid And SO3
pink, or the pH meter shows pH 7. Record the amount of NaOH
Molarity SO, in solvent = mis NaOH used / 40
So a 1-molar SO3 complex will require 40 ml of .IN NaOH to
neutralize it. Two equivalents of NaOH react per sulfuric acid.
If after 12 hours, the solvent has still not absorbed enough SO),
just let the process continue. The complex formed need not be exactly
.5M in acetonitrile, or 1 M in dimethlyformamide, just close to those
values. What is important is that the exact strength of complex formed
be known, because that dictates just how much of SOa solution is
used. That is crucially important to the success of the reaction.
When the SOa-solvent complex has reached the desired strength,
the flask containing it should be stoppered with a glass or Teflon
stopper, and kept in the fridge. It will gradually darken first to yellow
and then orange, but it is good for at least 3 or 4 months.
The argument can be made that this procedure is wasteful of
fuming sulfuric acid. After all, maybe only 2 liters of 1-molar SO3
complex can be reasonably made from a pint of fuming sulfuric acid
by this passive fume-absorption method. When one considers that this is
enough SO3 to make 3 million doses, however, such objections are silly.
With SO3 complex in solvent prepared and carefully standardized to
evaluate its exact strength, attention can be turned to LSD synthesis
using lysergic acid and SO3 complex. Exact weighing of ingredients,
and assuring that they are free from water are the two main concern