LSD synthesis from Ergotamine

[ieatfungi]

Yoyoyo could anyone perhaps assist me in locating some ergotamine tartarate or containing medicines in the U.S? Any assistance is appreciated

 

[amieri]

Yoyoyo could anyone perhaps assist me in locating some ergotamine tartarate or containing medicines in the U.S? Any assistance is appreciated

ieatfungiEver have any luck

 

[Sneaky.Base]

3 grams of lsd gives 20000 to 30000 doses , excuse my noob question, how did they separate this exact small quantity to blotter on 30000 doses?
Tnx for any reply

 

[amieri]

3 grams of lsd gives 20000 to 30000 doses , excuse my noob question, how did they separate this exact small quantity to blotter on 30000 doses?
Tnx for any reply

Sneaky.BaseBy making a solution in distilled water or ethanol.each 1/4"×1/4" tab of blotter can hold x amount of liquid

 

[Macondor]

Introduction View attachment 4053 ​

LSD is an unusually fragile molecule, and some comments are in order as to its stability and storage. As a salt, in water, cold, and free from air and light exposure, it is stable indefinitely. There are two sensitive aspects of its structure. The position of the carboxamide attachment, the 8-position, is affected by basic, or high pH, conditions. Through a process called epimerization, this position can scramble, producing isolysergic acid diethylamide, or iso-LSD. This product is biologically inactive, and represents a loss of a proportionate amount of active product. A second and separate point of instability is the double bond that lies between this 8-position and the aromatic ring. Water or alcohol can add to this site, especially in the presence of light (sunlight with its ultraviolet energy is notoriously bad) to form a product that has been called lumi-LSD, which is totally inactive in man. Oh yes, and often overlooked, there may be only an infinitesimal amount of chlorine in treated tap water, but then there is only an infinitesimal amount of LSD in a typical LSD solution. And since chlorine will destroy LSD on contact, the dissolving of LSD in tap water is not appropriate.

There are many synthetic methods developed and reported for the preparation of LSD. All of them start with lysergic acid, and for that reason, it has been listed as a Schedule III controlled drug, as a depressant, under Federal law. The amide lysergamide, a component of several varieties of Morning glory seed, is also a controlled drug and, by law, a depressant.

The extraction procedure of Ergotamine from tablets is the same as in this method.​

Equipment and glassware: View attachment 4051 ​

• Round bottom flasks (RBF) 500 mL and 100 mL;
• Ice water bath;
• Retort stand and clamp for securing apparatus;
• Magnetic stirrer with heater;
• Vacuum source;
• Rotovap machine;
• Flash chromatography kit;
• Buchner flask and funnel (large) 5 L [Schott filter may be used for small quantities];
• Laboratory scale (0.01 — 100 g is suitable);
• Glass rod and spatula;
• pH indicator paper;
• Drip funnel 100 mL;
• 100 mL x3; 50 mL x2 Beakers;
• Reflux condenser;
• Separatory funnel, 500 mL.

Reagents:​

• Ergotamine tartrate (ET) 10 g;
• Potassium hydroxide solution (KOH) 6.7 g in 100 mL H2O;
• Sulfuric acid ~100 mL 2.5 N (H2SO4);
• Diethyl ether (Et2O) ~200 mL;
• Ammonia (NH3) anhydrous ethanol solution 50 mL 15%;
• Aqueous ammonia (NH4OH) 50 mL of 1% + 200 mL 1 N;
• Diethylamine (Et2N) 7.1 g;
• Chloroform (CHCl3) ~350 mL;
• Phosphoryl chloride (POCl3) 3.4 g;
• Magnesium sulphate (MgSO4) anhydrous ~100 g;
• Hexane ~200 mL;
• Dry methanol (MeOH) ~100 mL;
• Dry d-Tartaric acid (0.232 g per 1 g of LSD base);
• Distilled water ~ 500 mL.

View attachment 4047 ​

9,10-Didehydro-N,N-diethyl-6-methylergoline-8β-carboxamide tartrate:
Boiling Point: N/A;
Melting Point: 200 °C;
Molecular Weight: 473.5 g/mole;
Density: N/A;
CAS Number: 17676-08-3.

Procedure​

d-Lysergic acid hydrate

A solution of 6.7 g KOH in 100 mL H2O, under an inert atmosphere and magnetically stirred, was brought to 75 °C, and 10 g ergotamine tartrate (ET) (1) added in 500 mL round bottom flask. The reaction mixture turned yellow as the ergotamine went into solution over the course of 1 h. The stirring was continued for an additional 3 h. The reaction mixture was cooled to about 10 °C with an external ice bath, and acidified to a pH of about 3.0 by the dropwise addition of 2.5 N H2SO4. White solids started to appear early in the neutralization; approximately 60 mL of sulfuric acid (H2SO4) was required. The reaction mixture was cooled overnight, the solids removed by filtration, and the filter cake washed with 10 mL Et2O. The dry solids were transferred to a beaker, suspended in 50 mL 15% ammonia in anhydrous ethanol, stirred for 1 h, and separated by decantation. This extraction was repeated, and the original decantation and the second extract combined and filtered to remove a few hundred milligrams of unwanted solids. The clear filtrate was stripped of solvent under vacuum, the residual solids dissolved in 50 mL of 1% aqueous ammonia, and this solution was acidified as before with 2.5 N H2SO4. The precipitated solids were removed by filtration and washed with Et2O until free of color. After drying under vacuum to a constant weight, there was obtained 3.5 g of d-lysergic acid hydrate (2), which should be stored in a dark, sealed container.​

View attachment 4048 ​

Lysergic acid diethylamide (LSD) free-base
A suspension of 3.15 g d-lysergic acid hydrate (2) and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring. With the external heating removed, there was added 3.4 g POCl3 over the course of 2 min, at a rate sufficient to maintain refluxing conditions. The mixture was held at reflux for an additional 5 min, at which point everything had gone into solution. After returning to room temperature, the solution was added to 200 mL of 1 N NH4OH. The phases were separated, the organic phase dried over anhydrous MgSO4, filtered, and the solvent removed under vacuum. The residue was chromatographed over alumina with elution employing a 3:1 C6H6/CHCl3 mixture, and the collected fraction stripped of solvent under hard vacuum to a constant weight. This free-base solid (3) can be recrystallized from benzene to give white crystals with a melting point of 87-92 °C.​

View attachment 4049 ​

Lysergic acid diethylamide (LSD) tartrate
This base was dissolved in warm, dry MeOH, using 4 mL per 1 g of product. There was then added dry d-tartaric acid (0.232 g per 1 g of LSD base), and the clear warm solution treated with Et2O dropwise until the cloudiness did not dispel on continued stirring (use 100 mL RBF in this case). This opaqueness set to a fine crystalline suspension (this is achieved more quickly with seeding) and the solution allowed to crystallize overnight in the refrigerator. Ambient light should be severely restricted during these procedures. The product was removed by filtration, washed sparingly with cold methanol, with a cold 1:1 MeOH/Et2O mixture, and then dried to constant weight. The white crystalline product was lysergic acid diethylamide tartrate with two molecules of methanol of crystallization, with an m.p. of about 200 °C with decomposition, and weighed 3.11 g (66%).​

View attachment 4050 ​

Repeated recrystallizations from methanol produced a product that became progressively less soluble, and eventually virtually insoluble, as the purity increased. A totally pure salt, when dry and when shaken in the dark, will emit small flashes of white light.​

Medicines containing Ergotamine View attachment 4052 ​

There is the list of medicine which are containing Ergotamine:

• Brand names: Belcomp-PB, Cafatine PB, Micomp-PB, Ergocomp-PB
• Contain: Belladonna/caffeine/ergotamine/pentobarbital systemic

• Brand names: Bellergal-S, Spastrin, Eperbel-S, Bellamor​
• Contain: Belladonna/ergotamine/phenobarbital

• Brand names: Cafergot, Cafetrate, Wigraine, Ercaf​
• Contain: Caffeine/ergotamine systemic

There are many different medicines that contain ergotamine. You can search on Amazon or other search resource in your country.
​

G.PattonBoss I buy a LSD solution, 100mg in 5ml of vodka and i want to store indefinitely. Have some questions..
-Is better in the freezer or in the fridge?
-Is neccesary to bubble argon or nitrogen to the solution and fill the empty top part of the dropper with the inert gas or vaseline or something like that?
-Put a few mg of EDTA?

Thanks!!!

I want to store for years.

 

[G.Patton]

Boss I buy a LSD solution, 100mg in 5ml of vodka and i want to store indefinitely. Have some questions..
-Is better in the freezer or in the fridge?
-Is neccesary to bubble argon or nitrogen to the solution and fill the empty top part of the dropper with the inert gas or vaseline or something like that?
-Put a few mg of EDTA?

Thanks!!!

I want to store for years.

MacondorKeep receptacle tightly sealed. Store in cool (use -17-20 *C freezer), dry conditions in well sealed receptacles.

 

[Macondor]

Keep receptacle tightly sealed. Store in cool (use -17-20 *C freezer), dry conditions in well sealed receptacles.

G.Pattonthanks man, so is not neccesary do anything of what i described?
The vodka solution hermetic in the freezer and nothing more?
If in the droper have a a little space with air because is not full is not a problem?

love

 

[G.Patton]

thanks man, so is not neccesary do anything of what i described?
The vodka solution hermetic in the freezer and nothing more?
If in the droper have a a little space with air because is not full is not a problem?

love

Macondor

so is not neccesary do anything of what i described?
The vodka solution hermetic in the freezer and nothing more?
If in the droper have a a little space with air because is not full is not a problem?

I think it would be enough.

 

[GhostBlack]

How can I create an inert atmosphere? What devices do I need?

 

[UWe9o12jkied91d]

How can I create an inert atmosphere? What devices do I need?

GhostBlackHere, I have illustrated a classic inert gas reaction setup. You can follow the flow of N2 to the condenser where it eventually gets pushed out, ensuring little to no oxygen can enter.The flow must be calibrated as such that nitrogen does not push out reaction products or solvents that we don't want pushed, to this a end a bubbler can be attached between the canister and flask to visualize the flow of gas.N2 is used in this way in official settings since it is readily available and cheap, but also light, so it needs to be flowing to not be replaced with athmospheric air.
We need only to use our imagination to apply this to our amateur setting.A gas that is inert and by contrast to N2 is much heavier is Argon, it is more expensive and is much rarer, but available.Argon can be used this way by only filling your reaction medium using a canister and optionally pulling a vacuum at the end of the condenser and refilling with argon.

 

[GhostBlack]

Here, I have illustrated a classic inert gas reaction setup. You can follow the flow of N2 to the condenser where it eventually gets pushed out, ensuring little to no oxygen can enter.The flow must be calibrated as such that nitrogen does not push out reaction products or solvents that we don't want pushed, to this a end a bubbler can be attached between the canister and flask to visualize the flow of gas.N2 is used in this way in official settings since it is readily available and cheap, but also light, so it needs to be flowing to not be replaced with athmospheric air.
We need only to use our imagination to apply this to our amateur setting.A gas that is inert and by contrast to N2 is much heavier is Argon, it is more expensive and is much rarer, but available.Argon can be used this way by only filling your reaction medium using a canister and optionally pulling a vacuum at the end of the condenser and refilling with argon.

UWe9o12jkied91dThank you very much for the information

 

[G.Patton]

How can I create an inert atmosphere? What devices do I need?

GhostBlackInert atmosphere synthesis and distillation

 

[Nicoino]

Could lysergic acid methyl ester be used instead of ergotamine?
Would the basic condition hydrolize the methyl ester?
If this works the rest of the procedure would be the same.
Using methyl lysergate would make LSD synthesis really user friendly and cheap.
Any advice is appreciated

 

[archae]

Could lysergic acid methyl ester be used instead of ergotamine?
Would the basic condition hydrolize the methyl ester?
If this works the rest of the procedure would be the same.
Using methyl lysergate would make LSD synthesis really user friendly and cheap.
Any advice is appreciated

NicoinoYes, you can hydrolize under the same conditions to cleave the additional groups

 

[Nicoino]

Yes, you can hydrolize under the same conditions to cleave the additional groups

archaeThanks for the confirmation, may try in the future when I will have some money to invest in the process

 

[ZACARIASKLK123]

@G.Patton

Hi, can ergotamine tartrate be changed for "Dihydro Ergotamine Mesylate --> 6190-39-2"?

Adjusting molar ratios and such (obviously).

Perhaps we would obtain Lysergic acid diethylamide (LSD) mesylate? Or am I wrong?

 

[G.Patton]

@G.Patton

Hi, can ergotamine tartrate be changed for "Dihydro Ergotamine Mesylate --> 6190-39-2"?

Adjusting molar ratios and such (obviously).

Perhaps we would obtain Lysergic acid diethylamide (LSD) mesylate? Or am I wrong?

ZACARIASKLK123

Hi, can ergotamine tartrate be changed for "Dihydro Ergotamine Mesylate --> 6190-39-2"?

Yes, you can

Perhaps we would obtain Lysergic acid diethylamide (LSD) mesylate? Or am I wrong?

You won't get LSD mesylate if just substitute ergotamine salt. You need to change acid in the last step. I'm not sure that you can get LSD mesylate in practice.

 

[HerrHaber]

Yes, you can

You won't get LSD mesylate if just substitute ergotamine salt. You need to change acid in the last step. I'm not sure that you can get LSD mesylate in practice.

G.PattonIf done the chemist way, it should end up with nor-LSD but not mesylate salt. Ssince the product is closer to neutral (amide) but more basic than LSD due to the fact that it has a proton instead of methyl on the quinoline moiety nitrogen atom.

 

[NoraJean]

Anyone know how to go about sourcing ergotamine?

 

[PlanckB1]

Hello,

What solvent would you use for the purpose of recrystalising the D-Lysergic Acid Hydrate? Would ethyl acetate be suitable?

I also have a similar question for the recrystallisation of the lysergic acid diethylamide tartrate if there are any other solvents which the salt would have similar solubility to methanol?

Thank you very much

 

[nutella]

@G.Patton can I use something other than diethyl ether (Et2O) in step 1 for washing? Thanks

 

[G.Patton]

@G.Patton can I use something other than diethyl ether (Et2O) in step 1 for washing? Thanks

nutellaDioxane and, probably, petroleum ether.

 

[nutella]

and for the d-Tartaric acid is 147-71-7 or 87-69-4 the correct CAS? Thanks

 

[G.Patton]

and for the d-Tartaric acid is 147-71-7 or 87-69-4 the correct CAS? Thanks

nutellad-tartaric acid cas 147-71-7
l-tartaric acid cas 87-69-4
easy to google