jacob019 (Hive Bee)
04-21-02 17:32
No 299942
      dirty MDP2P  Bookmark   

So I performed the oxone rxn on isosafrole.  When I was ripping the solvent off of the product it got way too hot and turned black oops, oh well.  I ended up with ~50g of glycol/epoxide/crap.  I went on to do the H2SO4 reflux.  Every thing went fine I think. (It's my first time)  It didn't clean up very much with NaOH washes.  It's VERY dirty.  But it does have hints of red even though it's black, and it smells fruity like burnt flowers.  It smells a LOT different than before.  I'm not sure where to go from here.  I've thought about vacuum distillation. Best idea no? Well no, my vacuum source only pulls 5" Hg.  It does lower the bp of safrole ~30 though.  Some advice would be greatly appreciated.  Thanks.
04-21-02 19:34
No 299999
      your vacuum  Bookmark   

If your going to vac distill your ketone, your going to need a lot more vacuum than what you have. Your ketone will polmerize at around 200c. Your going to need a pump that pulls ~28"hg or hiher. Do a search for refrigerator pumps or hvac pumps. How high was the temp when the epoxide turned black. Soiunds kinda strange.

We'll soon find out if I'm a chemist or not!
04-21-02 20:38
No 300029
      sodium bisulfite purification  Bookmark   

sodium bisulfite available from your local home brew shop, the search engine will answer the rest, and next time you stripping solvents use a water bath!
(Hive Addict)
04-24-02 03:02
No 300751
      ketone polymerized  Bookmark   

it got too hot the epoxide rearranged to the ketone which subsequently poloymerized......
(Pioneer Researcher)
04-24-02 04:35
No 300767
      Distillation  Bookmark   

You can distill your ketone at 20-30 mm Hg or even a bit more.
(I'm not Cheesie)
04-24-02 16:15
No 300978
      bisulphite-nope  Bookmark   

Just from experience, the crude ketone from and Oxone epoxidation/H2SO4 rearrangement has too much Isosafrole in it to form a ketone precipitate. Maybe cheese's run was different but VL is right on the money when he stated that your epoxide was thermally rearranged to Ketone with the exessive heat. The ketone is dark dark brown with a hint of red and does smell of ketone after being left out for a few minutes (after the more volatile Isosafrole evapps off leaving MDP-2-P smell). Chromic says that you can distill the crude ketone without a vacuum if it's born from the Oxone route, but cheese wouldn't risk it. Get a vacuum.

<Cheeseboy-a whiteboy with soul, like a black guy without soul
May De Sorce Bee Wit Chu-Always