Sorry - somebody else mentioned the paper but they’ve since deleted their response I suppose.
And while I understand your point about the nasty unknowns, I don’t really follow your logic. You are performing a chemical conversion, using a protic acid to isomerize what is essentially a terpene bonded to an aromatic ring. If you know anything about the reactivity of terpenes, you know that there are inherently going to be side reactions happening, meaning you are producing impurities you don’t know about anyway. Regardless, you will be smoking crude
Yes indeed, smoking crude with uknowns is definitely a bad idea but I do believe its slightly less of a bad idea than smoking crude with known baddies in it.
I’ve tried looking into what it could be that I’m smoking of course, unfortunately there is little research interest in it so I can’t even remotely claim it to be benign. However since my conditions are relatively mild, I do believe it to be on the level of a burnt attempt at a pot brownie.
Getting equipment and solvents to run a chromatography column and vacuum distillation are my top priorities but it looks like the slowboat from china is going to take a month to get here at least.
10 g CBD + 20 ml (10 ml 96% pure Ethyl alcohol + 10 ml distilled water) + 30 g Citric acid in a closed E-flask with magnet and placed on a magnetic stirrer with heating.
Reflux while stirring at around 70 degrees Celsius for 42 hours.
Beam tests 4-AP tests about every 12 hours.
Neutralization with med 60 ml distilled water + 3 g sodium carbonate, then with only distilled water til pH shows neutral.
A light yellow upper layer appears, which is decanted over to a small 100 ml glass beaker, and a small magnet is added, and the beaker is placed on a magnetic stirrer while heating to boil off the alcohol + water.
Temperature checked with IR-thermometer and the beaker is removedf when the temperature exceeds 110 C, where all water and alcohol should have been boiled off.
The result was 9 grams of a an amber-colored sticky substans. About 1 grams was removed and åplaced in a small vial and sent to a lab for GC analysis. And the analysis: 37% CBD + 24% D9-THC + 10% D8-ISO-THC + 2% D8-THC. So about 36% identified THC-isomers.
If the reflux time had been extended for some days then there would most likely had been less remaining CBD and more THC’s.
Just as an update - I’ve given up on citric acid a while ago. My main motivation for using citric acid in the first place was the accessibility but I couldn’t get it to produce anything remotely clean with similarly accessible solvents like water, ethanol or propylene glycol. My best run IIRC was something like 30% D9, 30% d8, 20% unreacted and the rest of it various cannabinoid junk (±20%/%, these are estimates based off TLC).
My first attempt with toluene + ptsa brought me to 80% d9 10% d8 10% unreacted, the plates came out clean, distinct and it was easy to work up to 95%+ D9 since then sooo yeah…
