Synthesis of LSD-25 from Lysergic acid monohydrate

[WillD]

1. A slurry of 3.15 g d-lysergic acid monohydrate and 7.3 g diethylamine in 150 ml of pure chloroform is heated for reflux.
2. After the lysergic acid is dissolved (a few min) cool the mixture down to where reflux has stopped by removing the heat.
3. Before the mixture cools any further 2ml of phosphorous oxychloride is added at such a rate as to give reflux (about 2 min).
4. In addition, reflux for 4-5 min further, until an amber-colored solution results.
5. Cool to room temp and wash the mixture with 200ml of 1M ammonium hydroxide.
6. The chloroform solution was dried with MgSO4 (this would have to be after separation), filtered, and concentrated by evaporation in vacuum under a temp of 38 *C (at no time let the temp go over 40 *C).
7. Dissolved the residue in a minimum amount of methanol and acidify with a freshly prepared solution of 20% maleic acid in methanol (not aqueous) to precipitate the LSD in its maleate form.
8. Filter the fluffy white needles, was with cold methanol and air dry to get 2.2 g of LSD that requires no further purification.

 

[Altair]

Can I use tartaric acid instead of maleic acid?

 

[HerrHaber]

Can I use tartaric acid instead of maleic acid?

Altairmost probably yes givven that you adjust to the appropriate molarity to have correct results... another point is that people use L-tartaric acid in order to obtain the D-LSD

 

[Katty Korner]

Question being where does one order phosphorous oxychloride.

At least in the US I believe it is highly watched for this reason, as well as being used for nerve gasses iirc

 

[HerrHaber]

Question being where does one order phosphorous oxychloride.

At least in the US I believe it is highly watched for this reason, as well as being used for nerve gasses iirc

Katty Kornerthis is a very good question indeed... In Europe say it's easyer to come across but still hard I had mine thrown away but someone who has it may be kind enough to send over a 5-10mL ampoule you have also a restriction on the diethylamine which is not a problem where I'm at... not to mention the main ingredient that I can't seem to come across no matter how hard I try (long tedious way to play around with bromocryptine got me hospitalized and the final Grignard followed by hydrolysis is insinuated but no actual writeup found)

 

[Katty Korner]

this is a very good question indeed... In Europe say it's easyer to come across but still hard I had mine thrown away but someone who has it may be kind enough to send over a 5-10mL ampoule you have also a restriction on the diethylamine which is not a problem where I'm at... not to mention the main ingredient that I can't seem to come across no matter how hard I try (long tedious way to play around with bromocryptine got me hospitalized and the final Grignard followed by hydrolysis is insinuated but no actual writeup found)

HerrHaberI am very much unsure, but i thought one could produce diethylamine from DEET, a very common insect repellant. This is likely limited to small scale though

 

[HerrHaber]

I am very much unsure, but i thought one could produce diethylamine from DEET, a very common insect repellant. This is likely limited to small scale though

Katty KornerI really doubt the insect repellant itself is useful or that a procedure was devised to hydrolise it in order to obtain diethylamine and the less interesting 3-methyl benzoic acid that could perhaps serve as reagent to some other chemistry. I am uncertain of what I said above so please verify but it's the only purpose I can think of (diethylamine is a watched precursor in the US but not where I'm at so I can get easily hold of some)

 

[archae]

I really doubt the insect repellant itself is useful or that a procedure was devised to hydrolise it in order to obtain diethylamine and the less interesting 3-methyl benzoic acid that could perhaps serve as reagent to some other chemistry. I am uncertain of what I said above so please verify but it's the only purpose I can think of (diethylamine is a watched precursor in the US but not where I'm at so I can get easily hold of some)

HerrHaberI have to disagree here. I've seen a number of procedures about this, using a base hydrolysis. This isn't very effective, but if one cannot get their hands on DEA it's a viable option. Here is a link to one such procedure, there's a bunch of sciencemadness threads as well.
https://www.reddit.com/r/TheeHive/comments/sdccnp

 

[HerrHaber]

I have to disagree here. I've seen a number of procedures about this, using a base hydrolysis. This isn't very effective, but if one cannot get their hands on DEA it's a viable option. Here is a link to one such procedure, there's a bunch of sciencemadness threads as well.
https://www.reddit.com/r/TheeHive/comments/sdccnp

archaeI can't deem to grasp what is there to disagree about since I only developed on the comment above.. diethylamine I can get freely without a licence and it isn't of any concern where I'm at.

 

[archae]

I can't deem to grasp what is there to disagree about since I only developed on the comment above.. diethylamine I can get freely without a licence and it isn't of any concern where I'm at.

HerrHaber"I really doubt the insect repellant itself is useful or that a procedure was devised to hydrolise it in order to obtain diethylamine" in your comment just above mine, where I shared a procedure that has been devised to hydrolise DEET into diethylamine.
If you can get diethylamine freely your luckier than most of us sadly

 

[HerrHaber]

"I really doubt the insect repellant itself is useful or that a procedure was devised to hydrolise it in order to obtain diethylamine" in your comment just above mine, where I shared a procedure that has been devised to hydrolise DEET into diethylamine.
If you can get diethylamine freely your luckier than most of us sadly

archaeI was probably to hasty in reading your post

 

[archae]

I was probably to hasty in reading your post

HerrHaberHappens to the best of us!

 

[mxtlrr_chem]

In Step 6, is evaporation en vacuo required, or is it possible to evaporate it via normal heating?

 

[archae]

In Step 6, is evaporation en vacuo required, or is it possible to evaporate it via normal heating?

mxtlrr_chemYes. It is used to removes oxygen from the reaction vessel and to lower the boiling point of chloroform so that it doesn't have to be heated as long or as strong as under atmospheric pressure.
LSD and its precursors is very reactive with oxygen and heat and readily undergo degradation if not handled properly.

 

[mxtlrr_chem]

Yes. It is used to removes oxygen from the reaction vessel and to lower the boiling point of chloroform so that it doesn't have to be heated as long or as strong as under atmospheric pressure.
LSD and its precursors is very reactive with oxygen and heat and readily undergo degradation if not handled properly.

archaeIt seems like it takes expensive equipment (rotovap) to perform this, at least from what I understand. Could this be done w/o a rotovap and placing your vacuum chamber in the heating?

 

[archae]

It seems like it takes expensive equipment (rotovap) to perform this, at least from what I understand. Could this be done w/o a rotovap and placing your vacuum chamber in the heating?

mxtlrr_chemyes, or you can just connect a vaccum pump to your drying vessel using a gas adapter

 

[chemistry.mob]

What is the CAS number of d-lysergic acid monohydrate?
thank you !!

 

[mxtlrr_chem]

What is the CAS number of d-lysergic acid monohydrate?
thank you !!

chemistry.mob82-58-6.

 

[csigger]

Can someone perform this synthesis? I believe I can obtain all the necessary chemicals for it. If someone can do it, I will provide all the chemicals needed. The recipe seems simple, although it's theoretically not. I'm hesitant to attempt it alone because the chemicals are very expensive. It would be one of the happiest days of my life if someone would collaborate with me.