pickler (Hive Bee)
02-13-02 16:47
No 269123
      Isosafrole atmospheric  Bookmark   

Swim usually makes his iso using vacuum, so swim decided to try it at atmospheric this time. Swim was refluxing it and getting about 1 drop a second. Is this sufficient to convert the safrole to iso? Swim was running it for 3 hrs.
Should swim have ran it longer?

We'll soon FIND OUT if I'm a chemist or not!
 
 
 
 
    LaBTop
(Daddy)
02-13-02 20:12
No 269207
      Re: Isosafrole atmospheric  Bookmark   

Swim obviously can't read. Try again reading the posts regarding this issue from the last days, there's no talk about refluxing, just heating to 120 to 160 C for at least 6 to 12 hours with 2 to 10 % KOH added to your distilled safrole. And then you don't get that ugly tar, you still get a blackish solution ofcourse, but no tar left after distilling your isosafrole out. LT/


WISDOMwillWIN
 
 
 
 
    Vibrating_Lights
(Hive Bee)
02-14-02 02:44
No 269389
      Re: Isosafrole atmospheric  Bookmark   

If you got it.   Bring your saf KOH up to boil under vac,  hold there for one hour.  then remove vac and bring up to reflux and hold it there till the tempat the base of the condensor is 254. then the hot plate to what temp your iso will boil under vac.  it is best to do this in one of the conical round botttoms as the distilling flask. hook the vac back up and with the adjustable regulator distill your iso.  this distillation can be done very quickly if you pay attention and are very cordinated. if it starts choaking let it off a  little.  if done correctly a steady stream of iso is possible.
VL_
 
 
 
 
    ChemicalSolution
(Hive Bee)
02-26-02 12:07
No 273731
      Re: Isosafrole atmospheric  Bookmark   

SWIM know's someone who did the KOH isomerization.  She refluxed under vac for 4-5hrs.  Almost NO safrole distilled over!!  It was (probably) >85% iso.

Julia
 
 
 
 
    noj
(Hive Addict)
02-26-02 13:55
No 273760
      Re: Isosafrole atmospheric  Bookmark   

What was the other 15%? Did you not use distilled safrole in the start?


Chaque un son gout
 
 
 
 
    psychokitty
(Her Majesty, Stoni's Kitty)
02-27-02 00:19
No 273984
      Re: Isosafrole atmospheric  Bookmark   

It would boil earlier than 254 C (which is the trans isomer bp--or is it?).  The cis isomer bp is around 243 C.
 
 
 
 
    Vibrating_Lights
(Hive Bee)
02-27-02 09:55
No 274155
      Re: Isosafrole atmospheric  Bookmark   

I believe that somewhere it has been said that even with the vaccume reflux almost everything is converted by the 3.5 hr mark.  the extended times just ensure high yeilds.
VL_
 
 
 
 
    cheeseboy
(cheese head)
02-27-02 22:35
No 274437
      Re: Isosafrole atmospheric  Bookmark   

LaBTOP--   Wouldn't heating for 6-12 hours be considered a reflux? Cheesemelty.

         May The Source Bee With You...Always.
 
 
 
 
    goiterjoe
(Hive Addict)
02-27-02 23:49
No 274479
      Re: Isosafrole atmospheric  Bookmark   

if the liquid doesn't reach it's boiling point, then it's not refluxing.

If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music