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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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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. After
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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