New LSD write-ups

prankster · Sat Jul 02, 2005 12:31 am

Well.
I see that alot of chemists are using beginning to use the peptide coupling methods.
afortunately if you need some info for this methods you need to search alot of website fora's and messageboards. There is no detailed write-up for these methods.
Only the first one wich was from rhodium New route from ET-->LSD
This isn't exactly the holy paper of lsd via Peptide coupling.

And after some reading on this Forum I get more and more confused.

The one method uses triethylamine, the other method uses different ccouplers at the same time. And their is almost no information about how much iso-LSD is produced. Because when your coupler gave you an 80% yield from which 50% is iso-LSD the after converting your iso-LSD to LSD you lost yet again some LSD and the total yield of pure LSD is still 60%.

Then with the POCl3 method people knew what to avoid and stuff. And the tips and tricks like avoiding H2O, Chlorine, O2, CO, bright light, high temps.

Don't have any off that with coupling methods. With coupling methods it something like this. 5 part of Pybop in 5 parts of DCM you add 5 parts of DEA in 5 parts of DCM which you add to 2 parts of LSA in 5 parts of DCM. (This is not real. Just an stupid example)

Well that is not exactly something to go on for the first time coupling chemist.

mk-1 · Sat Jul 02, 2005 4:56 pm

coupling of lysergamides is described very nicely in Nichols' paper about dimethylazetidines analogues of LSD-25. The group uses PyBoP as the copupler along with a weak base (diisopropylethylamine). coupling takes 3 hours and gives high yield.

here is a link -
http://rapidshare.de/files/2747172/lysergic_acid_isomers_of_2_4-dimethylazetidine_-nichols.pdf.html

prankster · Sat Jul 02, 2005 8:02 pm

Wow. Didn't know that one. That is a beautiful paper.

timnickbear · Wed Jul 06, 2005 1:39 am

would swin be able to take methanol and extract the la from hbwr and after using carbon and methanol to purify a little, seperate the la compounds in a prep column to get a layer of la to use in a cdi or pocl3 rxn to get small yeilds? this would be for a kilo or so of seed.

prankster · Sat Jul 09, 2005 5:45 pm

What I don't understand is the extraction and purification steps.

This is what they do

1:Extractions of layers with NH4OH and DCM
2:Washed 2 times with H2O and brine
3:dried with MgSO4
4:Filtration and Solvent removal by rotary evaporation under reduced light
5:Drying under high vacuum

This produced a light golden foam (Isn't LSD freebase a solid???? The solvent is removed, so I find that weird.)

6:purification by centrifugal thin layer preparative chromatography(4.1 DCM.hexane under N2 armosphere)
7:Then another Solvent removal in the dark (Do they mean the DCM from the chromatography????)
8:Then it is dissolved in tert-BuOH and combined with tartaric acid dissolve in a minimal amount oh propanol
9:This was stored overnight at 0 Celsius
10:Crystals were collected by filtration and dried overnight at 60 Celsius under high vacuum.

My questions are

1: Is LSD freebase a solid? And if so how can you have a golden foam when you have removed the solvent?

2:After chromatography the do a solvent removal. What solvent removal? Didn't they do that in step 4, or is it the DCM used during the chromatography??

3:What do the mean with drying under high vacuum?? Is that with a temparature or with a drying agent??

4:What for weird chromatography do they use. Is that do-able for a amature chemist?

5:Owsley III said that his Acid and truly good acid should be of 99.9% purity
In this paper they achieve a purity higher then 99%. But that can be 99.1% or 99.5%.
How can you proceed to make it even more pure then it already is???

6:They don't mention iso-LSD. Is this produced in the PyBOP method??

mk-1 · Sat Jul 09, 2005 8:42 pm

prankster, as i am not an lsd chemist, i can only answer from logic :
1 : it is logical to think that a product that comes out of the chormatography may not be in xtal form, until it is rextalized to form the xtals. it is possible to get a "foam". also remember that this is not LSD (lysergic acid diethylamide) but rather Lysergic acid dimethylazetidine. It has trhe same moeity as diethylamide. so it may have some other qualities.
2 : When u chromatograph you do it with solvents. meaning ull get your end product in one of the fractions which is the product with the solvent. it is required to remove the solvent in the end.
3 : drying under hugh vacuum means exactly what it says - drying the solid of solvent under HIGH vacuum to avoid using high temperatures.
4 : This chromatotron, is a kind of chromatograph tekinq. it uses a rotating disc, which rotates at high speeds. this disc is layed with silica (or alumina, just like a plate for tlc) and then it spins with differetn solvents creating several bands. it is a fast acting chromatography. for ametuer chromatogrpahy read up on column chromatography
5 : logic tells us, that you can either do another chromatography session, or u could simply rextalize alot. Shulgin in his book TIHKAL says that he chromatographs once, and then rextalizes several times to get the purest product.
6 : while it is true they dont mention iso lsd, it does not mean it does not form, though when u purify something in chromatogrpahy u seperate the iso from the non iso, so the final yield of the product is that of the "non iso" isomer.

loki · guinea pig

the drying under high vacuum means using a vacuum dessicator and a drying agent and the purpose is removing every last bit of water left in it

prankster · Sat Jul 09, 2005 11:47 pm

This is a quote from Bernard Roseman who manufactured LSD in the 60's

timnickbear · Sun Jul 10, 2005 2:54 am

Use a prep column and a vacuum flask to purify...you use dcm in the process and alumina activity of II-III. Look at windowlickers post. Make sure you have argon pref or nitrogen stream to avoid moisture. Maleic acid works better after the freebase is gotten to preserve the LSD.