Full disclosure: I bought these SOP’s and they were promised unlimited support and help when needed, this didnt work out and the author ghosted me and multiple others on this forum. So now that he can no longer offer the support and help as previously promised I am sharing these with the forum for all to enjoy and for anyone interested to give it their shot and share results and observations.
The first SOP is a revised version of the GLG Sulfur SOP
The second is a NO solvent SOP that requires sulfur and an addition of Iodine.
Enjoy and happy converting!
In the full spirit of the GLG I request that you keep this discussion moving forward with the goal for all to be able to make themselves or their labs some beautiful CBN isolate.
Disclaimer regarding trying to scale this reaction:
After reading through the solvent free reaction, the notes at the bottom say in case of a runaway reaction, place reaction flask into iced salt water. Am I crazy to think that would crack the flask immediately?
Borosilicate glasses are known for having very low coefficients of thermal expansion (≈3 × 10−6 K−1 at 20 °C), making them more resistant to thermal shock than any other common glass. Such glass is subjected to less thermal stress and can withstand temperature differentials without fracturing of about 165 °C (329 °F).
According to the reflux temp suggested in the SOP which is 180c then dropping into a salty ice water solution (approx -2c) would surely exceed that 165c differential.
lol @ “runaway reaction safety” on the neat reaction. The cyclization of CBD to THCs is exothermic and its super unwise to scale a neat reaction with a known exotherm - inherent process safety etiquette is to temper these types of things with solvent dilution. Specifically a solvent that has a boiling point that can absorb the exotherm. Not only is it dangerous, but that runaway exotherm contributes to an unknown impurity (in my experience). Big dick chemists don’t scale neat reactions.
Picking up an exotherming reaction is unwise, dumping hot glassware directly in cold anything is unwise. On scale, you might consider an “oh shit” lever where you flood your jacket with cold ass fluid and hope you don’t break your reactor.
I do think its dope you shared this with folks because maybe itll lead them to a smarter process solution quicker, I just hope they’re wise enough to take it with a grain of salt and not just dump this process into an across international 50L and hope for the best.
Don’t count on that flask holding up, and when the oil and water meet because the glass cracked, make sure your face isn’t over it. The last thing most people think about when an emergency arises, is a full face shield, but if you try to stop a reaction like that, you’ll need one.
I explicitly told the author I was inexperienced and wanted something safe and reliable. The more I learned back then the more flags that popped out. And now we’re here getting the input from multiple professionals which I’m sure will make this a safer experience for all involved.
Having had an exothermic reaction go wrong and come close to seriously hurting me (hyper-boiling 35% H2O2 exploded all over me), I can say that there will not be time to adorn one’s self with any additional PPE. Should add that step to the preparation part of the SOP.
Now that the equipment is set up and ready, prepare for imminent risk of danger by NOT DOING THIS REACTION!
I find the best way to knock some heat off of a reaction quickly is by using a battery powered leaf blower. Can drop a good 100c in a minute or two just blowing the air around the flask takes some btus off nice and quick.
Absolutely! Hopefully we can use this thread to share what works best for cleanup. I know once I get the time to play with this I can easily help dial in the clean up and will gladly share it with everyone.
I have successfully recrystallized cbn and isolated it from a sulfur smelling 83% oil. Once I get a little more crude built up I’ll gladly share a process for that after I have a few more repeatable runs to share.
(I’m not actively doing any conversions right now so it will be a bit before I can give it the attention it needs)