Theoretical synthesis of LSD from HBWR seeds

[MrChan]

Extraction:
1. Mix powdered seeds with acetone, more than enough to cover the top of the powder. Mix and let stand for 3 hours, filter off solution, repeat several times. I recommend filtering, washing and combining solvents in 2 different jars. Continue extracting until no more lsa comes out. You can use a uv black light to check each batch for lysergimides.

2.let solvent evaporate off at RT

3.mix in distilled water, and add enough citric acid to reach 4 ph, let sit for 5 minutes, filter again.

4.defat using naphtha, mix very well for 15 minutes, remove naptha and organic layer, repeat twice.

5.add ammonia .5ml at a time until 9ph

6. Add dichloromethane, stir for 20 minutes, separate dcm, let evaporate.

if you need a stopping point, skip evaporation and place Lisa/dcm mixture in cold dark place.

Hydrolysis of LSA:

1. Mix crystalline lsa in a beaker with distilled water and KOH, add glacial acetic acid dropwise until all lysergic acid precipitates from solution.

2.filter off lysergic acid, collect in a container, wash filter with dcm, add more acetic acid to filtrate to precipitate remaining LA, repeat filter washing.

3.dry solution, and work up.

/-/-/-/-/-/-/-/-/-/-
I won’t bother adding the final steps, since sir William has already been so kind as to put instructions here; I recommend pybop.

adapted from kash’s lsa guide

​

 

[Mango2cb]

Somethink is not working hiere. It was tried two times with 100 gram of Morning Glory and it didnt work - ended up with brown powder after filtration and it was not cristaline LSA. Maybe its not working with morning glory but it works with HBWR seeds? Can You please left info - somebody tried this? Also defating was tried as first with naphta and it still didnt work.

 

[davlovsky]

Somethink is not working hiere. It was tried two times with 100 gram of Morning Glory and it didnt work - ended up with brown powder after filtration and it was not cristaline LSA. Maybe its not working with morning glory but it works with HBWR seeds? Can You please left info - somebody tried this? Also defating was tried as first with naphta and it still didnt work.

Mango2cbFrom Uncle Fester:

...these seeds have a considerable amount of another type of alkaloid in them besides the ones that yield lysergic acid. These other alkaloids are of the clavine type, meaning that they have the lysergic-acid skeleton, but lack the carboxyl grouping. In its place will be a methyl grouping, an alcohol grouping, a methyl alcohol grouping or combinations of the above. These clavinet alkaloids will likely be carried all the way through into the product, producing both the GIGO situation during the synthetic operations and a contaminated
product when finished.

Anyway, from further reading, it seems like Naptha, Hexane, Petroleum Ether (not Ethyl Ether) or mineral spirits can be used for defatting, which is done immediately after you've ground the seeds up. They recommend some columnar container, not unlike a Soxhlet extractor, except for the defatting phase, you wouldn't be recirculating your solvent, i.e. you'd be using as much Napatha as is necessary until it leaves no residue upon evaporation, after passing through your ground-up seeds.

After this, it looks like they recommend a methanol, ammonia and chloroform mixture to extract out the lysergic amides, which should be protected from light. Shining a black light on the collection vessel will reveal the amides, which will fluoresce a bluish color.

For the amount of theoretical starting material (I think it was something like 200lbs) that they've outlined in the book, they recommend about 10 gallons of this solvent-basing agent mix, but I'm wondering if the Soxhlet extractor would be suitable to keep recirculating the solvent-basing agent combo, so you wouldn't have to use so much (someone who's more experienced here would probably know if this is feasible).

Anyway, I'd recommend using HBWR seeds. If I remember correctly, they're a bit more potent than the Morning Glory seeds. (Or better yet, get your hands on some ergotamine-containing tablets/suppositories to isolate the ergotamine and start your synthesis that way.)

What solvent-basing agent mix are you using to extract out the amides from the seeds?

 

[Mango2cb]

From Uncle Fester:

Anyway, from further reading, it seems like Naptha, Hexane, Petroleum Ether (not Ethyl Ether) or mineral spirits can be used for defatting, which is done immediately after you've ground the seeds up. They recommend some columnar container, not unlike a Soxhlet extractor, except for the defatting phase, you wouldn't be recirculating your solvent, i.e. you'd be using as much Napatha as is necessary until it leaves no residue upon evaporation, after passing through your ground-up seeds.

After this, it looks like they recommend a methanol, ammonia and chloroform mixture to extract out the lysergic amides, which should be protected from light. Shining a black light on the collection vessel will reveal the amides, which will fluoresce a bluish color.

For the amount of theoretical starting material (I think it was something like 200lbs) that they've outlined in the book, they recommend about 10 gallons of this solvent-basing agent mix, but I'm wondering if the Soxhlet extractor would be suitable to keep recirculating the solvent-basing agent combo, so you wouldn't have to use so much (someone who's more experienced here would probably know if this is feasible).

Anyway, I'd recommend using HBWR seeds. If I remember correctly, they're a bit more potent than the Morning Glory seeds. (Or better yet, get your hands on some ergotamine-containing tablets/suppositories to isolate the ergotamine and start your synthesis that way.)

What solvent-basing agent mix are you using to extract out the amides from the seeds?

davlovskyFor defating i was using naptha and it was working nice in the begining of reaction - it works better than doing it as a point 4 like on this writeup abowe. Than aceton to extract LSA and yes it was giving nice little green light when i was usin black UV light.

After i was trying going as in point 5 and hydrolisis. But what i ended up is not cristals but brown powder on paper filter.

Normaly i expect white product after acid base purification...

I ask because i have about 10 kilo of HBWR in total and i have to do somethink with it...Soxhlet extractor i think will be greate for this, i gues i have to try this out and check by myself. But than i think i need to find some way to get out cristaline product from aceton...And this is hard part i think...

 

[davlovsky]

For defating i was using naptha and it was working nice in the begining of reaction - it works better than doing it as a point 4 like on this writeup abowe. Than aceton to extract LSA and yes it was giving nice little green light when i was usin black UV light.

After i was trying going as in point 5 and hydrolisis. But what i ended up is not cristals but brown powder on paper filter.

Normaly i expect white product after acid base purification...

I ask because i have about 10 kilo of HBWR in total and i have to do somethink with it...Soxhlet extractor i think will be greate for this, i gues i have to try this out and check by myself. But than i think i need to find some way to get out cristaline product from aceton...And this is hard part i think...

Mango2cbAre you basifying with ammonia first before extracting with Acetone? I think generally you'll either use acidic acetone (e.g. acetone mixed with tartaric acid) or basified solvent (dcm, ether, etc. mixed with ammonia).

Here's another tek I found that might be more suitable for you:
Ground seeds were transferred to a flask and submerged in petroleum ether for defatting. The seeds and petroleum ether were mixed thoroughly for 5 hours. After this time, the seed residue was filtered out from the petroleum ether. The seed residue was then subjected to 3 separate washes. For each wash, the seed matter was mixed with a solution of acetone and tartaric acid for 1 hour and then filtered. The liquid filtrate from each wash was saved. After the third wash, the filtrates were combined and gently heated to expel the acetone. The resulting solution was then washed with ether 3 times and made basic by adding liquid ammonia until its pH was between 8 and 9. To extract the alkaloids from this basic solution, three washes were performed using dichloromethane. The dichloromethane portion from each wash was saved and combined together.

At this point though, when you have your DCM/alkaloid solution, I'm guessing you'd probably want separate using chromatography, or possibly, you could just evaporate it all off and see what you get.

I think the reason that HBWR or Morning Glory seeds aren't really feasible is the amount of starting material and solvent required to get a good yield, and how much purification is required, but IDK. I've seen a lot of teks online for LSA extraction and surprisingly, they don't seem to be that popular or successful other than for producing something very crude where the end result is to be consumed instead of being processed further into LSD.

My guess is that these clandestine LSD chemists have some source of lab-grade LSA, or they're starting with Ergotamine from these migraine medicines.

 

[HerrHaber]

As far as I know it's surprisingly unfeasible to convert this specific amide to the acid by conventional hydrolysis maybe check out some enzyme of some sort.

 

[Mango2cb]

Extraction:
1. Mix powdered seeds with acetone, more than enough to cover the top of the powder. Mix and let stand for 3 hours, filter off solution, repeat several times. I recommend filtering, washing and combining solvents in 2 different jars. Continue extracting until no more lsa comes out. You can use a uv black light to check each batch for lysergimides.

2.let solvent evaporate off at RT

3.mix in distilled water, and add enough citric acid to reach 4 ph, let sit for 5 minutes, filter again.

4.defat using naphtha, mix very well for 15 minutes, remove naptha and organic layer, repeat twice.

5.add ammonia .5ml at a time until 9ph

6. Add dichloromethane, stir for 20 minutes, separate dcm, let evaporate.

if you need a stopping point, skip evaporation and place Lisa/dcm mixture in cold dark place.

Hydrolysis of LSA:

1. Mix crystalline lsa in a beaker with distilled water and KOH, add glacial acetic acid dropwise until all lysergic acid precipitates from solution.

2.filter off lysergic acid, collect in a container, wash filter with dcm, add more acetic acid to filtrate to precipitate remaining LA, repeat filter washing.

3.dry solution, and work up.

/-/-/-/-/-/-/-/-/-/-
I won’t bother adding the final steps, since sir William has already been so kind as to put instructions here; I recommend pybop.

adapted from kash’s lsa guide

​

MrChanIn this movies I see similarities – the plan is to extract ergot alkaloids in similar way

Extraction of Claviceps purpurea Part 1

100 grams od claviceps purpurea was grinded and petroleum ether was added by heating in water bath. This step will defat the product before extraction. Tartaric acid in water was added + aceton (10 g tartaric, 50 ml water, 150 ml aceton) – this was left with seeds over night. Filtered solution was acidified by sodium bicarbonate.

Ergot: the story of a parasitic fungus (1958)

17.00 to 19.00 minute

EXPERIMENT (without defating)

75 gram od morning glories was grinded and sodium bicaronate 15g disolved in 100 ml of water was added, than add 200 ml of acetone. Than 10g of tartaric acid in 100ml of water was added and solution was shaked and mixed. Than sodium bicarbonate was added in powder until ph reach 6 (neutral). Mixture was left and yellow solids perticipated (0,6g) and was filtered – it should be (egotamine, ergosine, ergocornine, ergocriptine, ergocristine). Probobly ergometrin remains in aceton/water solution and can be extracted with chloroform. After concentration ergometrin should cristalise.

It looks nice and now I have to test this material, I don’t know if its stable– if You have any idea how should I do it – just write a comment. I will try this method with HBWR in bulk – minimum 1 max 5 kilo extractions and than I will inform about results in august I hope.

 

[Mango2cb]

EXPERIMENT 2 - WILL BE MADE ALSO ONLY WITH HBWR

https://chemistry.mdma.ch/hiveboard/tryptamine/000474518.html

1. HBWR Extraction - From Rec. Drugs by Prof. Buzz:
Pulverize the seeds in a clean blender until they are a fine powder. Put this powder into a beaker, add 1 1iter of petroleum ether to every 900 to 1000g of powdered seeds, stopper the beaker to prevent evaporation and let set for 3 days. Filter off the petroleum ether and let evaporate to make sure no amides were extracted (there should not be much, if any) from the ether. Add 1 1iter of methanol (dry is best) and let soak for 4 days with vigorous shaking, now and then. Filter off the methanol and evaporate it under vacuo (vacuum speeds the process). In the meantime, add 500 ml of fresh methanol to the powder and extract it again for 3 or 4 days.

Filter as before and extract again with about 300 ml of methanol. Combine the residues of all extractions and hydrolyze.

2. Obtain Lysergic Acid by Hydrolysis of #1 Product using Jacobs and Craig method:
1.0g of ergotinine(or in this case #1 Product) was dissolved in 20ml of N-methyl alcoholic KOH and the methanol was removed at once by distillation at low pressure. The residue was treated with 20ml of an 8% aqueous solution of KOH and the mixture was heated on a steam-bath for 1 hour. A stream of nitrogen was passed through the flask during the heating and basic volatile material from the reaction mix was collected by passing the gas through a solution of dilute HCl acid.

The alkaline solution was made acid to Congo red with sulfuric acid. At this point, a considerable amount of partly crystalline material precipitated. The acid suspension as such was placed in an extractor and exhaustively extracted with ether. The aqueous suspension which remained was then filtered. The dark colored solid was treated successively with 2x20ml portions of ammoniacal ethyl alcohol which left a residue which was inorganic. The filtrate on evaporation to dryness under reduced pressure gave a residue which was digested a short time with 5ml of methyl alcohol to remove colored impurities. After cooling, the undissolved crystals were collected. 0.26g of a slightly colored crystalline solid was obtained which melted with decomposition at 235°C.