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 Divinorium Lysergicaciddiethylamide 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
Forum Ayahuascayage or this reaction is about 25° C throughout.
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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@Thursday, September 20, 2018 11:15:58 PM