Looking for a workable D9 SOP for CBD isolate to D9, preferably without any metals. Need to have conversion in the 90’s with low D8
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Without metals hmm
Borontriflouride is your only option then
And getting 90 + is gona take a lot of solvent but yes doable
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I know I can use triiso to do this at a greater purity but the purple is what becomes the problem from what I have heard.
The only proven way is with Al(iBu)3. Beyond that, you’ll have to experiment with other lewis acids and solvents.
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I could get you most of the way there without metals and safe catalysts, but as others have mentioned, I’ve tried every ‘safe’ way of going about this and the only way to get to 90’s with selectivity for D9 is TIBA or BF3
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https://pubs.acs.org/doi/10.1021/acs.joc.3c00300
Haven’t seen this posted anywhere, seems relevant
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If anyone is interested in my triisobutylaluminium SOP feel free to DM me. It yields above 90% d9 typically. The lowest ive seen it yield is 85%. The purple color can be prevented from forming and the SOP is quite affordable.
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AlCl3 also goes to 90’s.
It’s cheap and much easier to handle, compared to TIBA or BF3.
Beside the solvent and AlCl3 on its own, everything else is food grade.
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Indeed !!! Nice find and honestly spot on
Finnaly a paper that has treu conversion numbers of the listed reagents I have tried 5 and the numbers claimed are very close to what I achieved
Spot on Great refrance 
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AlCl3 is comparable to triisobutylaluminium in d9 yield, but not at scale. I think the biggest batch ive heard of anyone yielding above the 80’s with AlCl3 is 10 kilos. Anyone looking for a fully scaled SOP that hits 90% or above should hmu
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hey is there any way i could peep that triisobutylaluminium SOP???
+90% D9 at 15kg batch size. Its scalable. But thats nothing you get without full understanding of the fundamentals.
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With Tiba It is not doable at Scale 8kg~85% d9 . Most because of intense drying of everything since any moisture leed to Creation of d8 and catalyst quench.
I Had No Problem hit 85+ d9 at 15 kg in 40min scale without any extensive workup. And for Sure this Numbers can be done better.
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Hmu in the DMs my man
I’m curious at what % you are using the AlCl3 in relation to the CBD. I believe our last bench top rxn we used 1% and it turned blood red so fast. It seemed to me that we used too much.
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That is a normal phenomen and no indicator for a completed reaction like it was used to with pTSA reaction. It will turn blood red straight away. It will turn golden/amber again when you quench the rxn
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Thank you so much for the info! We got overwhelmingly positive results confirmed via GC. I am super stoked to run another. My only question is: is there any other solvent than DCM that would be appropriate for this RXN? It just fucking blows that all of my o-rings on all of my QD fittings are nitrile. All of my tubing is fiber reinforced PVC. It’s starting to look like I need PTFE o-rings and nylon braided PTFE tubing.
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Only DCM so far
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Swap all your orings to kalrez and never worry again (;
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