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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
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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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the alumina, two zones that fluoresce blue can be spotted by
illumination with a black light. The faster-moving zone contains LSD,
while the slower-moving zone is iso-LSD.
When the zone containing LSD reaches the spigot of the burette, it
should be collected in a separate flask. About 3000 ml of the 3-1
benzene-chloroform is required to get the LSD moved down the
chromatography column, and finally eluted.
The iso-LSD is then flushed from the column by switching the
solvent being fed into the top of the column to chloroform. This
material is collected in a separate flask, and the solvent removed
under a vacuum. The residue is iso-LSD, and should be stored in the
freezer until conversion to LSD is undertaken. Directions for this are
also given in this chapter.
For the fraction containing the LSD, conversion to LSD tartrate
must be done to make it water soluble, improve its keeping
characteristics, and to allow crystallization. Tartaric acid has the
ability to react with two molecules of LSD. Use, then, of a 50% excess of
tartaric acid dictates the use of about 1 gram of tartaric acid to 3
grams of LSD. The three grams of LSD would be expected from a
well-done batch out of a total 3.5 LSD/iso-LSD mix.
The crystalline tartrate is made by dissolving one gram of tartaric
acid in a few mis of methanol, and adding this acid solution to the
benzene-chloroform elute from the chromatography column.
Evaporation of the solvent to a low volume under a vacuum gives
crystalline LSD tartrate. Crystals are often difficult to obtain. Instead,
an oil may result due to the presence of impurities. This is not cause
for alarm; the oil is still likely 90%+ pure. It should be bottled up in
dark glass, preferably under a nitrogen atmosphere, and kept in a
freezer until moved.
If chromatography reveals that one's chosen cooking method
produces little of the iso products, then the production of the tartrate
salt and crystallization is simplified. The residue obtained at the end
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of the batch is dissolved in a minimum amount of methanol. To this is
then added tartaric acid. The same amount is added as above: one gram
tartaric acid to three grams LSD. Next, ether is slowly added with
vigorous stirring until a precipitate begins to form. The stoppered flask is
then put in the freezer overnight to complete the precipitation.
filtering or centrifuging to isolate the product, it is transferred to a dark
bottle, preferably under nitrogen, and kept in the freezer until moved.
LSD from (so-LSD
Two variations on this procedure will be presented here. The first is
the method of Smith and Timmis from The Journal of the
Chemistry Society Volume 139, H pages 1168-1169 (1936).
The other is
found in US patent 2,736,728. Both use the action of a strong
hydroxide solution to convert iso material into a mixture that contains
active and iso material. At equilibrium, the mixture contains about 2/3
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put into a 500 ml flask along with a solution made up of 150 ml ethyl
alcohol, 150 ml water, and 100 grams KOH. Next, 15 ml of hydrazine
hydrate is added. This hydrazine should be the monohydrate, which is
64% hydrazine. If a weaker variety has been scrounged up, this can be
made to work by adding more, and using less water.
Now the flask should be fitted with a condenser, and flushed with
nitrogen. Then heat the flask in an oil bath to gentle boiling for 4
hours. A slow stream of nitrogen to the flask during the reflux averts
the danger from hydrazine.
The flask is next cooled, and the contents poured into a sep funnel of
at least 1000 ml capacity. The batch is then extracted with 600 ml
ether, followed by 600 ml of an 85-15% mix of ether and alcohol.
Finally, one more extraction with 600 ml of 85-15% ether-alcohol is
All of the desired product should now be extracted into the
solvent, and out of the water. This fact should be checked using a
black light to look for the characteristic blue fluorescence.
The combined solvent extracts should now be lowered to a pH of
about 2 using HC1. At this point, a precipitate should form, and it
should be filtered out. The precipitate should be washed free of
entrained product with 4-1 ether-alcohol, and the washing added to
the rest of the filtered solvent.
Now 2750 ml of water should be added to the solvent, and the
mixture placed in a gallon and a half glass jug or 5000 ml beaker. To
this should be added 3 portions of cation exchange resin in H* cycle.
Cation exchange resin is a common item of commerce used in
deionized water systems. Check the yellow pages under "water" and
see which of the local Culligan men offer deionized water systems.
The deionizers come in two-tank systems with one tank packed with
cation exchange resin to remove calcium, magnesium and sodium
from the water. The other tank has an anion exchange resin to remove
chlorides, sulfates, and so on. It is no great task to buy cation
exchange resin from these outlets. The resin consists of tiny plastic
beads coated with the exchanger. In the case of the cation exchangers,
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this is generally a sulfonate. "In H* cycle" means that the resin is
charged up and ready to go. This is generally done by soaking the
resin in 20% sulfuric acid in water for a while, then rinsing with
distilled water. Check the directions on the container of resin. Steer
clear of mixed resins that contain both anion and cation exchangers. If
the Culligan man is too stupid to know the difference, or doesn't
know what he has, keep looking until you find one who knows his
The treatment with three portions of cation exchange resin in H*
cycle should be done as follows: Each portion of resin should weigh
about 15 grams. The first portion is added, and then the mixture
should be stirred strongly or shaken for about 10 minutes. The product
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@Tuesday, September 25, 2018 5:46:30 PM