Hello all, one of my colleagues introduced me to this site and said I would find a plethora of skilled consultants.
I am looking for an SOP on the conversion of CBD to D9 using TiBA. Will happily pay for consultation. I understand most of it. I know how to handle/transfer pyro chems. Will be working in glove box with nitro and cannula transfer through a septum. I understand dissolving CBD in heptane/hexane and adding tiba in hexane stirring for 12 hours at 25C and then quenching dropwise with water in a chilled environment. Celite, and recovery then distillation.
Even still I would really appreciate someone more knowledgeable than I to hold my hand through the process and verify my procedures. Like I said, will pay.
I could see the dilution in ether as a safety precaution before the quench, you think the addition of salts is necessary even at 19% tiba concentration in hexane?
yes yes ok I understand that. My main priority is the quench. I have been using water…VERY slowly and one of my colleagues said that this was not the correct way to do it and that I should seek consultation…so here I am.
Well welcome to the forum my lady
As for consultation I hate to say it but @roiplek is skilled
I would also recommend contacting trescolabs in Germany and check out there non pyrophoric reagents
As for quenching DRY alcohols with a base work fine
Also swap nitro for argon
And place a h2so4 moisture trap on your sparging gear
Ooo ok if you can Handel Raney this is. A walk in the park
I would recommend doing dcm solvent to get the drill then swap to pentane if your gear can be cooled to catch the exotherm
There is one isseu with tri thou
The colour remediation of your end product is
Crucial so who ever you hire make sure he s got that solved
Don t mind helping out but I am a cook and you have probably more chemistry background than me
Making a consult on a chemistry gig some what weird
I ll send a dm in case you can t
Be safe
Yes that’s the thingy there are quenches that take care of this and will give an amber/gold oil
One of the main reasons several like boron trifluoride more
As for the purple other than the right quench
Many run this on heptane and forget that Triiso should not be heated over 72C for it disintegrates so never reflux over 68C (reason I love hexane
Bu-Li compounds are probably the worst to deal with among the aluminum containing compounds.
Chemistry for other purposes provides a ton of potential routes for quenching such reactions.
A few things are universal:
Lower the temperature as much as possible (some procedures recommend a dry ice/isopropanol slurry).
Dilute with the appropriate solvent. Some work ups recommend slowly adding isopropanol, then methanol, then the water. Lots of waste just to not generate violent results.
Edit—just want to note in the posted procedure. They say that this procedure is only recommended for volumes of less than 20mL of t-BuLi and that the quenching has to happen in a vessel that is at least 1L!!!
