Hawaiian Baby Woodrose Seeds
ing in the cold before then adding 25 ml of diethylamine.
Stir for an additional 10 minutes, then pour the batch into a 2000
ml sep funnel. Now to the sep funnel add 800 ml of water. Mix this in
thoroughly, then add 400 ml of saturated salt solution in water. Mix
this in, then extract out the LSD by repeated extraction with 250 ml
portions of ethylene dichloride. Check with a blacklight for complete
6 LSD From Lysergic Acid And SO3
The combined ethylene dichloride extracts should be evaporated
under a vacuum as above, and the residue of LSD and iso-LSD should be
separated and treated as above.
LSD From Lysergic Acid And
LSD From Lysergic Acid
And Trifluoroacetic Anhydride
This method is a little bit lame, but it may be the method of choice if
trifluoroacetic anhydride or trifluoroacetic acid should happen to fall
from the sky into one's hands. The reason why this method is a bit lame
is threefold. Anhydrous lysergic acid is required for this reaction. To
obtain anhydrous lysergic acid, the lysergic acid hydrate yielded by the
methods in Chapter 5 must be baked under high vacuum for a
couple hours. This is obviously not good for such a delicate molecule.
The water molecule will be shed by a baking temperature of 120° C at a
vacuum of 1 mm Hg, 140° C at 2 mm Hg, and still higher
temperatures at less perfect vacuums. A MacLeod gauge is the only
instrument that I know of which is capable of accurately measuring
such high vacuums.
Another reason why this method is lacking is that the yields are
not so good as those achieved by the other synthetic routes presented in
this book. It is possible to recover the unreacted lysergic acid at the end
of the process, but this does not make up for the initial lower yield,
not to mention the added hassle of recovering and redrying the lysergic
Strike number three for this route is its propensity to give byproducts
that are difficult to separate from the desired product. I am
Practical LSD Manufacture
not talking here about the large amount of iso-LSD that this method
makes. That molecular jumbling is inconsequential, because the
lysergic acid used is itself an isomeric mixture. Rather, what can
occur here is the production of LSD and other by-products.
The mechanics of this reaction are similar to the reaction with
SOs, in that two molecules of the anhydride react with the lysergic
acid molecule to form the mixed anhydride. In this reaction, there is
no need to first react the lysergic acid with hydroxide to form the
metal salt. Also, the need to follow exact stoichiometric quantities of
reactants is not as pressing as in the SO$ method.
To do the reaction, into a 1000 ml flask (carefully dried and
equipped with a magnetic stirring bar) place 16 grams of lysergic acid
and 375 ml of acetonitrile. The lysergic acid will not dissolve. Stopper
the flask and place it in the freezer to cool the contents to -20f
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When all the methyl nitrite has been bubbled into the reaction
mixture, stirring should be continued for another hour. Then, if
palladium bromide was used, it should be filtered out. Repeated
filtrations will be needed to remove all of the catalyst, because it gets
quite finely divided during the course of the reaction. This leaves a
clear light-reddish solution. If palladium bromide was used, now
adjust pH to 4-7, and allow another hour to complete the hydrolysis.
If palladium chloride or the mixed catalyst was used, these
substances are soluble in alcohol. In this case, the catalyst will be
recovered later. Here, check the pH of the solution again to be sure it is
in the proper range before proceeding.
Now the alcohol solvent must be removed. This is best done by
pouring the reaction mixture into a large filtering flask, stoppering the
top of the flask, and removing the solvent under a vacuum. Use of a
hot-water bath to speed evaporation is highly recommended for this
process. It is not OK to distill off the alcohol at normal pressure, as
the heat will cause the nitrite and NO in solution to do bad things to the
To the residue left in the flask after removal of the alcohol, add
some toluene to rinse the product out of the flask into a sep funnel.
Next, put 300 ml of water into the flask to dissolve the catalyst if
PdCla or the mixed catalyst was used. Add the water solution to the
sep funnel to dissolve carried-over catalyst there, then drain this water
12 Studies On The Production OfTMA-2
solution of catalyst into a dark bottle and store in the dark until the
next batch. If PdBr2 was used, this step can be skipped. Just store the
filtered-out PdBra under water in the dark.
Now the toluene-phenylacetone solution should be distilled
through a Claisen adapter packed with some pieces of broken glass to
effect fractionation. The first of the toluene should be distilled at
normal pressure to remove water from solution azeotropically. The
b.p. of the azeotrope is 85° C, while water-free toluene boils at 110° C.
When the water is removed from solution, turn off the heat on the
distillation, and carefully apply a vacuum to remove the remainder of
the toluene. Then with the vacuum still on, resume heating the flask,
and collect the substituted phenylacetone. Methylenedioxyphenylacetone
distills at about 140° C and 160° C using a good aspirator
with cold water. A poor vacuum source leads to much higher
distillation temps and tar formation in the distilling flask. The yield
from the reaction is close to 150 ml of phenylacetone. Its color should be
clear to a light yellow. The odor of methylenedioxyphenylacetone is
much like regular phenylacetone, with a trace of the candy shop odor
of the safrole from which it was made.
A higher-boiling phenylacetone like 2,4,5-trimethyloxyphenylacetone
is better purified as the bisulfite addition product, unless a
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alkaloids, to unreacted lysergic acid, or lysergic acid hydrazides to iso-
LSD and God knows what substances created by the mishandling of
the raw materials and product, a contaminated product is much easier to
make than a pure one.
The use of large volumes of solvents poses twin problems:
obtaining them and disposing of them. Both problems are made vastly
Practical LSD Manufacture
simpler by recycling the solvents. Just because a solvent has been
used once in a given stage of the process does not mean its useful
lifetime is over. For example, the solvent used for defatting the crop is
easily made as good as new by distilling it to free it of its load of fat.
Other solvents are not so easily recovered for re-use because the
procedure calls for the given solvent to be removed from the product
by vacuum evaporation. In this case, the solvent can be collected in a
cold trap placed along the vacuum line on its way to the vacuum
source. If a pump is used to create the vacuum, such a trap is vital to
prevent solvent vapors from getting into the pump oil, thereby ruining
the lubrication and the vacuum created.
A cold trap can be constructed of either glass or steel; it need only be
large enough to hold the solvent collected, and airtight so as not to ruin
the vacuum with leaks. This cold trap is then cooled down with dry ice
during vacuum evaporations to condense the solvent vapors in the trap.
The solvent recovered in the trap can be re-used in the given stage of
the process from whence it came. I would not co-mingle recovered
solvents from different stages. For example, chloroform from the
alkaloid extraction of the crops should be kept for that usage, and not
be used for LSD crystallization, because it will also contain some
ammonia and methanol.
The recovery of ether, for example, from method 2 of lysergic acid
production, poses a special problem. This problem is the formation of
explosive peroxides in ether during storage. Ether containing water
and alcohol, as would be the case for this recovered solvent, does not
form much peroxide. There is a possibility that dry ether can be made
free of peroxides by shaking the ether with some 5% ferrous sulfate
(FeSO4) solution in water prior to distilling. Failure to do this may
expose the operator to a fiery explosion during distillation. Ice water
flowing through the condenser, and an ice-chilled receiving flask, are
required to get an efficient condensation of the ether during
Keeping Out Of Trouble 71
Keeping Out Of Trouble
The dangers of LSD manufacturing do not end with the possibility
that the cooker may spill some of the stuff on himself and fry his
brain. There is a much more malignant danger facing those who
embark upon this course: Johnny Law.
The conduit through which those shit-eating dogs travel to get to
you is your associates. If you are cooking alone with no partners in
crime, your safety has been impro
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into the benzene during separation pour everything back into the separator, let it
stand and repeat the separation more carefully. It is better to leave some
benzene layer in the water and emulsion than to get emulsion and water into the
benzene. Nothing will be wasted. All of the benzene which contains the
mescaline will eventually be salvaged. Sometimes the layers will fail to separate
properly. If this is the case immerse the funnel or jug in a deep pot of hot water
for two hours. This will break up the emulsion and bring about the separation.
Prepare a solution of 2 parts sulfuric acid and one part water. (never add water to
the acid or it will splatter; add the acid a little at a time to the water by pouring it
down the inside of the graduate or measuring cup containing the water.) Add 25
drops of the acid solution one drop at a time to the benzene extracts. Stopper the
jug and shake well for one minute. Then let stand for five minutes. White streaks
of mescaline sulfates should begin to appear in the benzene. If these do not
appear, shake the jug more vigorously for two to three minutes and let it settle for
five more minutes. I have found that when extracting mescaline from San Pedro
it is sometimes necessary to shake the mixture more thoroughly and for a longer
time to get the mescaline streaks to form. This is probably because of the lower
mescaline content in the plant. This would also apply to any peyote that does not
have a high mescaline content. After the streaks appear add 25 more drops of
the acid solution in the same manner, shake as before and let settle for ten
minutes. More streaks will appear. Add 15 drops of acid, shake and wait 15
minutes for streaks to form. Add 10 drops, shake and wait about 30 minutes.
Test the solution with wide range pH paper. It should show that the solution is
between pH 7.5 and 8. Allow the mescaline sulfate crystals to completely
precipitate. Siphon off as much of the benzene as possible without disturbing the
crystals on the bottom of the jug.
The next steps are to salvage any mescaline still in the water and emulsion layer.
Combine the benzene siphonings with the water/emulsion layer, shake these well
together for 5 minutes and let settle for two hours as before. Carefully remove the
benzene layer, treat it again with acid, precipitate the crystals and siphon off the
benzene as in the previous steps. Recombine the siphoned benzene with the
watery layer and repeat this again and again until no more crystals precipitate.
Siphon off as much benzene as possible without drawing crystals through the
The next step involves removing the remaining benzene from the crystals. There
are two methods to choose from. The first is the quickest, but requires ether,
which is dangerous and often difficult to procure. Shake up the crystals with the
remaining benzene and pour it into a funnel with filter paper. After the benzene
has passed through the filter rinse
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