SIMPLIFYING LSD SYNTHESIS
Cornholio
typical LSD synthesis? This simplfies the procedure considerably , and
reduces the amount of equipment/chemicals needed.
Attached is a typical LSD synthesis, based on Hoffman's original LSD
patent, which is also attached at the end of the file, so you can compare
if you want.
If you leave out the chromatic adsrobtion, you will be left with
approximately 50-66% d-LSD and 33-50% iso-LSD in the final product. instead
of just plain d-LSD, the active entheogen. This would weaken the final
product by weight since the isomer, iso-LSD is not psychoactive. You would
then need to increase the weight dose of your product in order to make up
for this.
As an example, in the following synthesis, leave out STEP 4, and increase
the concentration of the solution used in STEP 6 to 100mg/ml.
TYPICAL LSD SYNTHESIS
DO THIS ALL UNDER UV LAMP ONLY, LSD IS LIGHT SENSITIVE
STEP 1: convert ergot alkaloid (LSA, lysergic acid) into its hyrazide
you can obtain the LSA alkaloid from extraction of morning
glory seeds or HAWAIIN baby woodrose seeds with ether,
cultivation/extraction of ergot fungus and extraction with ether, or
acquisition of
actual lysergic acid (ergotamine)
SKIP DOWN TO 1) IF YOU ALREADY HAVE ERGOTAMINE(LSA)
FOR SEEDS/FUNGUS DO THE FOLLOWING
they're (LSA, other ergot alkaloids) soluable in non-polar "oily" solvents
like ether,benzene or chloroform, not polar solvents like water
crush the seeds or ergot fungus up in water and make a mush
mix in the "oily" solvent (ether,benzene,or chloroform),
shake well (a stoppered roundbottom flask works nice for this)
let the liquid settle, it will seperate into two layers(phases),
you want the upper "oily", "non-polar", layer.
Siphon or pour it off. (better yet use a seperatory funnel)
The lower, "watery", "aqueous", layer can be discarded
filter the alkaloids (LSA) from the oily layer using a coffee filter or
vacuum filtration with a buchner funnel
let the crystals dry, then use them
1) in a roundbottom flask mix 1 volume powdered ergot LSA alkaloid (or
ergotamine) and 2
volumes anhydrous hydrazine
2) add 2 volumes distilled water and boil for 15 minutes
3) cool in the refrigerator to get isolysergic acid hydrazide
STEP 2: convert the hyrazide to its azide
and convert the azide into the acid
use an ice bath, chill reagants for this step
1) dissolve 3 g lysergic acid hydrazide rapidly in 100 ml 0.1N HCl
2) 100 ml 0.1 N NaNO2 is added after 2-3 minutes vigorous stirring.
3) 130 ml more HCl is added dropwise
4) stir again
5) After 5 minutes neutralize to ph7 with NaHCO3
6) extract with 300 parts ethyl-ether
7) remove aqueous solution
8) dissolve gummy substance (isolysergic acid azide)
in ether
9) dry with freshly calcinated pottasium carbonate
10) add 3g diethylamine per 300 ml ether extract
allow to stand in dark 24 hours with repeated shaking
11) evaporate in vaccuum ---> isolysergic acid diethylamide
12) add 30 parts distilled water, filter
STEP 3: convert isomer
1) allow the solution to stand for several hours in 4N alcoholic
pottassium hydroxide
2) Neutralise with dilute HCl
3) make slightly basic with NH4OH
4) extract with chloroform
5) Evaporate in vacuo
this converts it into equal parts of isomers iso and d-lysergic acid
diethylamide
STEP 4: seperate isomers using chromatic adsorption
1) dissolve mixture in chloroform containing 0.5% ethanol, 1g/50ml
2) pass through column containing aluminum oxide (60cm longx4cm radius)
and chromatogram developed with the same solvent.
soak the column then drain
3) The dark impurities pass rapidly into filtrate. -> discard
4) Then follows a bright zone (blue appearance under UV light) containing
d-lysergic acid diethylamide from this 1.0-1.3 parts will be
obtained.
5) a further third slower passing portion contains the isomer (0.8-1.2
parts) strip the column with MeOH to quicken third pass, convert isomer
again as in
STEP 3, then repass through column
STEP 5: make the acid salt
1) dissolve one equivalent of the base with one equivalent d-tartaric acid
in a small quantity of methanol, the neutral tartrate crystallizes
out.
STEP 6: apply to blotters
1) make a 50 mg/ml solution of LSD tartrate from STEP 5 in isopropyl
alcohol
in otherwords put 5 gram LSD into 100mll isopropyl alcohol in a 250ml
beaker
2) dip 10x10 sheets of blotter into the beaker
3) drain, place on wax paper or aluminum foil to dry
4) wrap the dried sheets in aluminum foil
as cited
U.S. Patent 2,438,259; Patented Mar. 23, 1948. UNITED STATES PATENT OFFICE
2,438,259 d-LYSERGIC ACID DIETHYLAMIDE Arthur Stoll and Albert Hofmann,
Basel, Switzerland, assignors Sandoz Ltd., Fribourg, Switzerland, a Swiss
firm. No Drawing. Application April 28, 1944, Serial No. 533,264. In
Switzerland April 30, 1943 1 Claim. (CI. 260--236) The present invention
relates to new d-lysergic acid dialkylamides which are valuable therapeutic
products and to a process for their preparation. It has been found that by
condensing azides of d- or d,l-lysergic acid respectively or of d- or
d,l-isolysergic acid respectively or mixtures of these compounds with
diakylamines, d-lysergic acid dialkylamides are obtained, which products
have not yet become known hitherto. The alkyl groups present in the
dialkylamines used according to the present invention can either be
identical or different and may be of saturated or unsaturated character.
Such amines are for instance dimethylamine, diethylamine, dipropylamine,
dibutylamine, diamylamine, methyl-ethylamine, ethyl-allylamine,
butyl-amylamine, etc. The new d-lysergic acid amides are distinguished from
the known natural and synthetic ergot alkaloids and from the d-lysergic
acid amides described in our U. S. Patent No. 2,090,430 by their powerful
specific action on the central nervous system. The condensation of the
d-lysergic acid- or d-isolysergic acid azides with the dialkylamines is
carried out in the presence of an inert organic solvent and preferably at
room temperature. During the reaction taking place between the azides and
the dialkylamine generally mixtures of different dialkylamides will be
obtained. This can, for instance, be seen in the following illustrative
example showing the reaction of d-lysergic acid azide with diethylamine.
During the interaction of these compounds a mixture will be obtained
consisting of d-lysergic acid diethylamide and of d-isolysergic acid
diethylamide, from which mixture the d-lysergic acid derivative will be
separated. By using as a starting product d-isolysergic acid azide and
diethylamine a mixture of d-lysergic acid diethylamide and of d-isolysergic
acid diethylamide will be obtained, this mixture being subsequently
separated into its constituents. Finally by starting from racemic lysergic
acid azide or racemic isolysergic acid azide, mixtures consisting of
d,l-lysergic acid diethylamide and d,l-isolysergic acid diethylamide will
be obtained, from which the d-lysergic acid diethyl amide can be separated
in a suitable manner, e.g., in form of its tartaric acid salt. The
following examples, without being limitative, illustrate the present
invention, the parts being by weight. Example 1 3 parts of d-isolysergic
acid hydrazide are transformed in the usual way in a hydrochloric acid
solution by a treatment with sodium nitrite at 0 degrees C. into the azide,
and, after neutralization of the acid solution with sodium bicarbonate, the
azide thus formed is shaken out by means of 300 parts ethyl ether. The
ethereal solution is then dried with freshly calcinated potassium carbonate
and treated with 3 parts of diethylamine. The solution is allowed to stand,
preferably in the dark and at room temperature, for 24 hours with repeated
shaking. The ether is then evaporated in vacuo, the residue triturated with
30 parts of water and filtered by suction. The dark amorphous product thus
obtained possesses a specific rotation of [alpha]20/D=about+100 degrees (in
pyridine) and consists essentially of a mixture of nearly equal parts of
d-lysergic acid diethylamide and d-isolysergic acid diethylamide. The
separation of both isomers can be carried out for instance by the so-called
chromatographic adsorption method. For this purpose the mixture is
dissolved in chloroform containing about 0.5% of ethanol and is passed
through a column of aluminium oxide of 60 cm. length and 4 cm. radius and
the chromatogram developed with the same solvent. The dark impurities pass
rapidly into the filtrate. Then follows a bright zone, which has a blue
appearance in ultra-violet light and which contains the d-lysergic acid
diethylamide. From this fraction 1.0 to 1.3 parts of this product will be
obtained. A further slowly passing portion of the solution contains the
d-isolysergic acid diethylamide. By evaporating this chloroform fraction
and crystallizing the residue from acetone, 0.8 to 1.2 parts of a compound
crystallizing in beautiful prisms of melting point 182 degrees C. (corr.)
under decomposition is obtained, this compound being the pure d-isolysergic
acid diethylamide. Its specific rotation is [alpha]20/D=+217 degrees (c=0.4
in pyridine). Elementary analysis has given the following values: C 74.41;
H 7.48; N 13.27%. The calculated values for d-isolysergic acid
diethylamide, i.e., C20H25ON3 are C 74.25; H 7.79; N 13.00%. The
d-isolysergic acid diethylamide can be transformed into d-lysergic acid
diethylamide by using the methods known for the ergot alkaloids. By
allowing the solution of the iso- compound to stand in dilute alcoholic
potassium hydroxide, a mixture of about equal parts lysergic acid and
isolysergic acid compounds will be produced after a short time. The
d-lysergic acid diethylamide can then be separated from the mixture in the
manner described above. The amorphous d-lysergic acid diethylamide, which
can be separated by the chromatographic method, crystallizes, by dissolving
it in a small amount of acetone and diluting this solution with ethyl
ether, in bundles of needles. From benzene pointed prisms will be obtained,
that melt under decomposition at 80-85 degrees C. (corr.). The new compound
is difficulty soluble in water, but very soluble in methanol and ethanol.
It possesses the specific rotation of [alpha]20/D=+30 degrees (c=0.4 in
pyridine). Elementary analysis gives the following values: C 73.50; H 7.81;
N 12.92%. For d-lysergic acid diethyl amide, C20H25ON3, the calculated
values are C 74.25; H 7.79; N 13.00%. By dissolving one equivalent of the
base with one equivalent of d-tartaric acid in a small quantity of methanol
the neutral tartrate of d-lysergic acid diethylamide crystallizes out in
form of bundles of needles. The salt is very easily soluble in water and
melts indistinctly and under decomposition at 200 degrees C. (corr.).
Example 2 An ethereal solution of d-lysergic acid azide, prepared in the
usual manner from 3 parts of d-lysergic acid hydrazide, is treated with 3
parts of diethylamine and allowed to stand for 24 hours in the dark and at
room temperature with occasional shaking. The isolation of the compound
thus produced is carried out in the manner described in the Example 1. The
first separation by means of the chromatographic adsorption yields 1.3 to
1.7 parts of d-lysergic acid diethylamide and about 0.5 to 0.8 part of
d-isolysergic acid diethylamide. Example 3 3 parts of racemic isolysergic
acid hydrazide are transformed in the usual manner into the respective
azide and the formed compound is precipitated by means of an excess of a
sodium bicarbonate solution in the form of voluminous yellowish flocks,
which are separated by suction and immediately introduced at -5 degrees C.
into a solution of 3 parts of diethyl amine in 30 parts of ethanol. The
azide readily dissolves in the solution which becomes brown and is then
heated slowly to 30 degrees C. The solution is maintained at this
temperature for 1 hour, whereupon the solvent is evaporated in vacuo. The
sticky residue is triturated with 30 parts of water and filtered. The raw
condensation product amounting to about 2.8 parts consists of racemic
isolysergic acid diethylamide and of racemic lysergic acid diethylamide and
is separated by the chromatographic method in the manner described in
Example 1. During the chromatographic separation two zones are obtained
which are colored, in ultra-violet light, in brilliant blue shades. The
more rapidly passing zone contains the racemic lysergic acid diethylamide,
whereas the slower passing zone consists of racemic isolysergic acid
diethylamide. From the racemic lysergic acid diethylamide the d-lysergic
acid diethylamide can be separated by transforming the same for instance
into its neutral tartaric acid salt. For this purpose 3.2 parts of racemic
lysergic acid diethylamide (1/100 mol.) are dissolved in 6 parts of
methanol and added to a solution of 0.75 part of d-tartaric acid (1/200
mol.) in 2 parts of methanol. On inoculation with d-lysergic acid
diethylamide tartrate this compound crystallizes out in nearly colorless
bundles of needles. Yield 1.0 to 1.2 parts. The properties of the compound
thus obtained are identical with those described in Example 1 for the
neutral d-tartaric acid salt of d-lysergic acid diethylamide. What we claim
is: The crystalline d-lysergic acid diethylamide which crystallizes from
benzene in prisms melting with decomposition at 80-85 degrees C., which is
difficulty soluble in water but easily soluble in methanol and in ethanol,
which possesses the specific rotation [alpha]20/D=+30 degrees (c=0.4 in
pyridine) and which corresponds to the formula C20H25ON3. ARTHUR STOLL
ALBERT HOFMANN REFERENCES CITED The following references are of record in
the file of this patent: UNITED STATES PATENTS Number............
Name..........................Date 2,090,430....... Stoll et
al.............Aug.17, 1937 2,265,207....... Stoll et al.............Dec.
9, 1941 2,265,217....... Stoll et al.............Dec. 9, 1941
Cornholio
nosp...@my-deja.com
squi...@echelon.alias.net (Cornholio) wrote:
> Is it feasible to leave the chromatic adsorbtion speration out of a
typical
> LSD synthesis?
Yes, in large scale synthesis of LSD the use of chromatographic
separation is not advised. It is better to use fractional
crystalization. With the use of tartaric acid, d-lysergic acid
diethylamide is crystalized from methanol as the tartrate and
isolysergic acid diethyalamide remains in the mother liquor. In the
presence of strong base like potasium methoxide, isolysergic acid is
equilbrated back to a an equilibrium mixture of d- and isolysergic acid
diethylamide so a second crop of crystals can be recovered. In a
continous lab operation, the recovery of a second crop of crystals can
be made to coincide with the workup of a second synthesis so in the
long run, practically all isolysergic acid diethylamide can be
recovered as d-lysergic acid diethylamide tartrate.
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Before you buy.
sabertooth
Aahhh..theres nothing like the smell of
ergotamine tartrate in the morning...
Smells like shit but there nothing like it..
--
s a b e r t o o t h
picloud
<nosp...@my-deja.com> wrote in message news:8oltdj$lmr$1...@nnrp1.deja.com...
> In article <4f37bc8fb3d42a66...@anonymous.poster>,
> squi...@echelon.alias.net (Cornholio) wrote:
> > Is it feasible to leave the chromatic adsorbtion speration out of a
> typical
> > LSD synthesis?
>
> Yes, in large scale synthesis of LSD the use of chromatographic
> separation is not advised. It is better to use fractional
> crystalization. With the use of tartaric acid, d-lysergic acid
> diethylamide is crystalized from methanol as the tartrate and
> isolysergic acid diethyalamide remains in the mother liquor.
do you know why this happens??