If you pressurized and achieved 110oC or around toluene reflux could you do the procedure in ethanol or some ‘nicer’ solvent?
For the crystallization of CBN what do you use? Pentane has worked well but if there is a better dual solvent like Pentane/ethanol you can suggest?
Also for the d10 catalyst I know that a fire retardant was the first catalyst. Its definitely moved from there but I haven’t looked into it further.
Btw if anyone wants help operating a flash chromatography column I can help. There are a couple tricks that might save you some time. A big one is how to tell when you solvent mix is off after 10 runs.
It doesn’t work, as someone else mentioned that stoichiometry doesn’t add up. If you want to make CBN your starting material should be thc not random cannabinoids. If you want to do the iodine method there’s a whole paper on it and it’s not the way he describes it.
For what its worth, if anyone is still confronting this synthesis, I have a scalable high-yielding procedure for CBN synthesis and isolation. Slide me a DM, whomever.
The SOP is $15k and then there are hours of planning and training in addition to that. There are also various equipment requirements (like a fume hood, reactors, material handling, etc).
Iirc I was told oxone makes a lot of byproducts. But it’s hard to imagine a nastier process then sulfur. I’ve used oxone on other substrates, it’s convenient but it’s solubility causes annoying problems, you usually are working with a thick slurry and it requires strong overhead stirring.
if it works it works, but I have not come across another process pushing the same conversion as the process I use. We see 90+% conversion in the reactor, and downstream purification is a breeze because of that. I have no experience with oxone, but I can confirm that sulfur is definitely not the way to go.
Anyone reading that feel free to use oxone and report your findings. Make sure you bake the oxone and don’t expose it to water. Be careful, take proper precautions including ppe, have a plan for a runaway reaction and something handy to neutralize acids in case you come into contact. Always lle before distillation after you alter ph with acidic compounds (oxone) and make sure your water is coming out neutral
