quantum
(Hive Bee) 05-08-03 08:26 No 432063 |
NaOH is not a good way to isomerize safrole | Bookmark | ||||||
well i have finaly got around to making another batch of ketone. did the bisulfite test and yep we got ketone. things I have noticed are that my ketone this time was green and not a light yellow. mag stirring is essentual it not only saves you a heap of energy in not having to shake the fuck out of your solution but trust me it saves glass. I have been through so many rb flasks condensors ect becouse of overhead stiring or manual shaking. never again. I have also come to the conclustion that NaOH sucks arse bad I have done veriose isomerizations with NaOH and KOH now and this is what I have found. NaOH + CaO (CaO was CaOH dried in a test tube at 1000 C) in isopropyl alcohol: this is probably the best way to do an iso with NaOH I got a 60% yeild and found you didont have to dry your alcohol just make sure your CaO is not CaOH no alcohole: no good the CaOH eats all of the safrole and you have a bitch of a job getting it back. no CaO in alcohol: i got no iso from this it was just to hard to control water content. no alcohol under vacuum for 12 hours: I got a 20% yeild not worth it for me. KOH: first try 90% yeild did it under vacuum with mag stirrer on never use NaOH again trust me the chem supplier is not going to suspect a thing if you ring them up and order KOH just tell them you drying grapes into raisens :) e3500 console login: root bash-2.05# |
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MTM (Hive Bee) 05-09-03 15:25 No 432309 |
NaOH is not a good way to isomerize safrole | Bookmark | ||||||
So this is some kind of basic research, but I fear it is no news at all. Use CaO/KOH and you are fine. UTFSE, there is a lot of info on this topic. M T M |
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