Let me see that Chromatography once you finish your Rxn you might be a little disappointedā¦
Im sure ill be fine.
It might take a few tries but I bet I can get similar results
Everything will be confirmed by @kcalabs
Just remember academics lie a lot on papers too Theyāre just trying to finish their PhD in 5 years instead of 6 lol
Yeah, I havenāt had much luck over the years with reproducing published work. Neither have many others -a study concerning the reproducibility of the top 25 cited cancer papers only found a few that were reproducible.
Anyway, I really donāt like the amount of pTSA they are using. Crazy amount. But maybe at RT that is key.
I gave it a try and did a small batch.
pTSA in anhydrous Toluol for 46h at RT with max stirringā¦
I have no COA, but my TLC shows only one spot at d8 reference.
The distille is rock hard. So, looks like I made high d8 instead of d9.
I dried everythink except of the pTSA monohydrate. I assume that the residual water amount lead to the high d8 amount.
Does anybody know how to dry the pTSA efficiently?
I would try to put it in Vac chamber with CaCl2.
They used monohydrate ptsa
Did you use inert atmosphere?
They did
I inerted with Argon, yes
My pTSA was pink and clump.
It could definetly be dryer.
Iāve never seen pink ptsa Mines a white clumpy crystal that easily dissolves
pTSA will turn a bit pink if stored under mild heat and vacuum -in my experience anyway. Hopefully, that isnāt due to degradationā¦ but my slight pink pTSA still works well for d8. Maybe the pink comes from some loss of the water (monohydrate) upon being stored in dry conditions?
How big of a run did you do?
really? that was the first one i tried right when the paper was posted:
77% d9
11% d8
1000mg scale
and with dcm got 94% d8 and .1% d9 just like the paper
Did you run it the exact same way as the paper?
Im trying 1% ptsa
yes with 2 mol eq
Hey guys just a quick question, i got hit with some waxy isolsteā¦not sure exact % but i know its present maybe in a 5-10% overall content?
How bad of an impact would this have on a cbd to d9 conversions regarding side reactions and what notā¦
I have some of @ZenLion material im running
I tried to make D8 and the reaction didnāt go off because of the fats and lipids (the cbd crystallized in my reactor over night after the reaction)
So even 5% wax in cbd isolate can ruin the entire reaction? Do you think it can cause side reactions?
Did you notice any other issues?
Only information I have is anecdotal and from one experience so take it with a grain of salt.
I did one rxn with waxy isolate and it was subjectively very weak.
Youāre gonna have to winterize before or after anyways. So why not just winterize before.
I ran the exact conditions like mentioned in the paper, but scaled it up to 10 gramms CBD in the run. It was distillate and no isolate.
I havenāt expected to reach that high d9 number from the paper in the first run, but to end up with nearly pure d8 is really confusing.
I ordered some CaCl2, will dry out the pTSA and give it another try, to see if residual water is the reason.
Deleted