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#
 
 
 
 
    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