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lt-up pressure from the flask. If the
stirring bar bangs too violently in the flask, remove it with a magnet
rather than break the flask.
Pour the contents of the flask into a 250 ml sep funnel, and drain
the lower layer (water solution of lysergic acid hydrazide tartarate)
into a 250 ml Erlenmeyer flask wrapped in foil. To the ether layer still in
the sep funnel, add 50 ml fresh decimolar tartaric-acid solution, and
shake. Examine the water layer for the presence of lysergic acid
hydrazide with a black light. If there is a significant amount, add this
also to the Erlenmeyer flask.
Place the magnetic stirring bar in the Erlenmeyer flask, and stir it
moderately. Monitor the pH of the solution with a properly calibrated
pH meter, and slowly add .5M (20 grams per liter) sodium hydroxide
solution until the pH has risen to the range of 8-8.5. Higher pH will
cause racemization. The freebase is then extracted from the water
solution with chloroform. Two extractions with 100 ml of chloroform
should complete the extraction, but check a third extraction with the
black light to ensure that most all of the product lysergic acid
hydrazide has been extracted.
The chloroform extracts should be evaporated under a vacuum in a
500 ml flask to yield the product. This is best done by rigging the 500
ml flask for simple distillation, and applying an aspirator vacuum to
remove the chloroform. Assume that the yield from this procedure will
be about 5 grams of lysergic acid hydrazide if ergot was the crop used.
Assume that the yield will be about 7.5 grams if seeds were used.
The difference here is due to the fact that in ergot, the amides
LSD Directly From The Lysergic Amides —
The One Pot Shot
are largely composed of substances in which the portion lopped off is
about as large as the lysergic acid molecule. Seeds tend to be more
conservative as to their building upon the lysergic molecule. A careful
weighing on a sensitive scale comparing the weight of the flask before
and after would give a more exact number.
Both of these choices are really very poor, because lysergic acid
hydrazide, unlike most other lysergic compounds, crystallizes very
well with negligible loss of product. At the hydrazide stage of LSD
manufacture, one has a perfect opportunity to get an exceedingly pure
product, freed from clavine alkaloids and other garbage compounds
carried in from the extraction of the complex plant material.
I refer the reader to US patent 2,090,429 issued to Albert
Hofmann and Arthur Stoll, the dynamic duo of lysergic chemistry,
dealing with lysergic acid hydrazide. In this patent, they describe in a
rather excited state how they were able to produce pure lysergic acid
hydrazide from tank scrapings that were otherwise impure junk.
Lysergic acid hydrazide has the following properties: it dissolves
easily in acid, but is very difficultly soluble in water, ether, benzene
and chloroform. In hot absolute ethanol it is slightly
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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
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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