The Real Peter Parker
Well-Known Member
I'm interested as well.
PCP and LSD recipe
- Thread starter blaznb
- Start date
dontexist21
Well-Known Member
Yup no joke, the guy was working on a experiment using reagents that he had previous experience with. The problem with the reagents are that they produce both H2 and heat in substantial quantities. So you have to go extremely slow while working with it. He though he was at the point where he was safe and hurried it along. Next thing he knows there is large explosion, his whole work area blows up. Glass from around him goes through his neck, blood was everywhere. I have two professors that knew two different people that this happened to.
Don't fuck around with Organic Chemistry, a lot of the reagents will either burn you, give you cancer, or blow up in your face. I almost caused a fire in my lab when I handled a compound I was not familiar with. Thankfully someone caught my mistake. My prof. once told me Organic Chemistry is a unforgiving bitch.
Edit: Just remembered both scientist were using Lithium Aluminum Hydride (LiAlH4), which is a very powerful reducing agent.
Brevity, The Soul Of Wit!
New Member
Oh, right, they weren't synthesizing LSD, I get it. But WOW that sucks.
The Real Peter Parker
Well-Known Member
Haven't seen blaznb post for a while... Maybe he was the first decapitated in LSD synthesis. From the egg, red wine, and cherry mix.
Brevity, The Soul Of Wit!
New Member
That was a really funny post. 
dontexist21
Well-Known Member
Sounds like someone is baking a cake, mmmm I like cake.
Brevity, The Soul Of Wit!
New Member
A cherry cake with wine for flavor...
The Real Peter Parker
Well-Known Member
And LSD between the egg whites.
Brevity, The Soul Of Wit!
New Member
Suuurrrre...
The Real Peter Parker
Well-Known Member
Hey I tried the recipe. It works. I'm trippin' balls. The problem is the wine. I'm not trippin as hard cause I used the 'milk carton' wine.
Brevity, The Soul Of Wit!
New Member
You mean box wine?
The Real Peter Parker
Well-Known Member
Yes, but a cheaper grade than even what you show in your picture.
Brevity, The Soul Of Wit!
New Member
I know. 
This is more like it....
This is more like it....
boristheblade
Member
albert h had a one pot shot method .i have it thanks to uncle fester . its not a one pot method at all .if i can figure out how to post it i will
The Real Peter Parker
Well-Known Member
Yeah. [ten characters]I know.
This is more like it....
Brevity, The Soul Of Wit!
New Member
Uncle Fester's a moron.
Albert Hofmann was a Swiss chemist who worked at a Swiss pharmaceutical company and had a reputation for being exceptionally thorough.
His method wasn't random but precise. They were controlled tests. Also known as EXPERIMENTS.
K?
shepj
Oracle of Hallucinogens
Agreed, Fester is a douchebag.Uncle Fester's a moron.
Albert Hofmann was a Swiss chemist who worked at a Swiss pharmaceutical company and had a reputation for being exceptionally thorough.
His method wasn't random but precise. They were controlled tests. Also known as EXPERIMENTS.
K?
ayo Brevity, you wouldn't happen to know where the tek Hoffman used is eh? I would love to see the comparison between Hoffman & Shulgin's synthesis (I would imagine it's a totally different ball game)
Brevity, The Soul Of Wit!
New Member
These are the methods of synthesis that Hofmann submitted to Sandoz for patenting I believe.
LSD-25
U.S. Patent 2,438,259; Patented Mar. 23, 1948.
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
Do these help??
LSD-25
U.S. Patent 2,438,259; Patented Mar. 23, 1948.
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
Do these help??
Brevity, The Soul Of Wit!
New Member
Yep yep yep. Important to note that it's not the exact method used for the first LSD synthesis. But the second synthesis used for Bicycle Day is here.
