I’m new to cannabis science but have lots of experience with CPC and am trying to develop an economically viable separation that yields pure d8. I am looking for reaction conditions that provide a messy d8 mixture so I can use it as a starting point challenge. I will be getting my hands on a distillate soon and (almost) have a fully functioning lab, but only understand the underlying theory of the conversions. It seems most posts here are trying to get clean conversion to d8, but nobody reports their procedures for making “less-than-ideal” mixtures.
I found the recent Journal of Natural Products post that seems to suggest dichloromethane with camphorsulfonic acid is good for the one to one mix of d8 and d9, so that will be my first foray, but I’d like to develop a separation that can deal with any possible d8-dominant input material.
So I guess what I am saying is can anyone provide procedures that will reliably/reproducibly give me decent yields of d8 with various impurities? The greater variety of selectivities, the better! I’ll gladly talk shop about CPC in exchange for any interested parties.
one should always strive to make the purest product possible, but in the name of science ill tell you what not to do.
forgo any inerting, run your reaction “open” to the atmosphere.
use a very strong acid, Muriatic was mentioned, and it yields pretty nasty stuff. Sulfuric, or HCL would also be good contenders, especially when you don’t take additional post and pre processing steps to ensure a clean reaction.
dont wash your material post reaction
dont filter your material post reaction
dont Distill your material post reaction, one could even distill and simulate a leak, imo this is where alot of unknowns are produced, the long retention time in an SPD coupled with improperly removed catalysts will absolutely destroy your “clean” product.
there are many ways where you could fuck up your product intentionally. just do everything you shouldnt do. it should go without saying, but im going to say it anyway. DONT DO ANY OF THE ABOVE TO MATERIAL THAT IS DESTINED TO BE FOR HUMAN CONSUMPTION.
If there is a messy sample you can probably run a few samples at various dilutions through LC/MS and GC/MS and just compare the peaks against a known NIST library, purely for an identification purpose.
There may be a few compounds difficult to identify this way but this might be a good start.
My apologies, just to be totally clear, I’m specifically looking for conditions that contain substantial quantities of d8. The majority of these articles do lend great insight into the variety of compounds that you can get, so I am definitely using them. The most compelling way to have control, it seems to me based on the article, would be to make each of the individual possible impurities and then combine the proportions I need.
Thank you, this is excellent bad advice. And I wholeheartedly agree with your adding the disclaimer. I am hoping to really come up with something that protects consumers in the long run.
(Just a heads up that muriatic acid is hydrochloric acid!)
reusing recovered solvents without purification and drying would also be an excellent variable to explore aswell. I bet at every stage of solvent reuse, you would see an additional increase in impurity formation.
Would be interesting to add a known amount of every isolated cannabinoid to your CBD to make a pseudo crude mixture, test the composition, then run the reaction and compare.
If you specifically added different amounts of each cannabinoid you may be able to loosely discern what’s happening to several of them. I suppose you could add some terpenes that would still be found in the starting material. Caryophyllene oxide, guaiol, etc is usually still in distillate. That will make things real messy though.
I will echo what others have said and say get lots of air involved. That’s going to be a big factor that will mimic what a lot of the novice conversions are creating.
Be safe tho. Not everyday people say “how can I do everything wrong” so this obviously will pose new risks that we might not be thinking about.
Interesting to see that they had no reaction with citric acid + EtOH at RT. I can confirm that you will get reactions with long reflux time (36h) at boiling temp (~45% totals incl. ~25% DT9, ~5% DT8, ~15% DT10), results according to external lab HPLC analysis. But it’s not possible to get much higher, and usually less than that. But it’s probably the safest method.
pTSA + Toluene at RT reflux 48h have so far resulted in the highest conversions, but so far not higher than ~85% in totals of DT9 and DT8.
I’m currently testing CSA + Toluene at different temps and reflux times. Has anyone else tried this and can present results?
