LSD tartrate salt formation problems

[Nicoino]

Hi guys, I'm really struggling to form the tartrate from the freebase.

This was my third trial, the first two were kinda messy and solvent probably not anhydrous, the amount of tartaric was also eyeballed to prevent losses from transferring the freebase flakes in a container to be weighted. I think the formation of hemi and ditartrate could have inhibited each other crystallization, so for my last try, stechiometric amounts were used.

I started with 1060mg of cream colored freebase which was dissolved in 4ml of anhydrous warm methanol, 245mg of tartaric acid were added and dissolved in a few seconds. Solution was stirred for a few minutes then ether was added dropwise ensuring the precipitate caused by a drop dissolved before another one was added.

Very slowly the solution got cloudy, a few more drops were added and solution was kept stirring for a few minutes.

After 10 minutes I checked on the process and sadly as happened on the other past failed runs an oily residue

precipitated with no crystal whatsoever. If anyone has any advice it would be immensely appreciated.

Attached below the photo of the freebase.

 

[testint]

Why you got some balls bro trying to tartrate your whole batch instead of small fractions ,crystallization can be finicky as you know and only three tries you sir are a gentleman and a scholar
Much respect

 

[VeNoMxXx]

Well Sounds like a Bit less Liquid for Convert to Salt methanol dry away to fast i would try with clean water/methanol and a little heat is needed work in Dark then it Start glow orange when it become tratrate Salt

 

[ViezeGrey]

Hello, have you had any success since your initial post?

I am at a similar stage, however instead of a residue I have graduated to a highly viscous "jelly like" formation, which I have not been able to crystallize into a solid structure. I attempted evaporating some of the solution to reduce the proportion of methanol however this did not effect. On a different note, did you reach your freebase form via the PyBOP reaction? Or another reaction?

 

[VeNoMxXx]

do you have accesss to a spectrometer anywhere ? from what is the freebase made or isolated ? LSD is high class chemistry its not cooking meth haha

 

[VeNoMxXx]

just Pm me if u need support may i can help u with it ! best regards

 

[VeNoMxXx]

i made LSA tratrate not sure how different it act in converting to salt , i used Alcohol/and clean water not sure what proportions exactly but it worked good after add tratratic acid slowly with a little heat it startred glow orange in the dark thats sign for radiation whats allways there with acid. how did u fully do it was it sure oil and water free ?