strangespice (Stranger)
05-28-00 03:44
No 10191
      Alfred makes MDP2P via novel path?  Bookmark   

Batman, having come to the cave early one evening, finds Alfred cranking the Bat-Hyvac for all its worth, distilling the final traces of his clandestine work.

After running the chagrined Alfred back to his quarters, Batman accidentally finds the notebook his hapless butler has dropped.....

Page 1

" This lunatic at the hive told me that I could degrade this bromosafrole to an alcohol by a short reflux in an equimolar amount of base in alcohol as a solvent, which I did.....
this same freak swears that you can now oxidize this alcohol to mdp2p in high yields with....

ohmygod  *

DMSO in NaOH?????????????????


Batman frowns and mulls this one over ....

Hive brains, CAN dmso in the prescence of base, oxidize a secondary alcohol to methyl ketone?


*&^%$#
 
 
 
 
    strangespice
(Stranger)
05-28-00 10:06
No 10267
      Re: Alfred makes MDP2P via novel path?  Bookmark   

according to a college text by Cram and Hammond, in the 50's, this can work......

Page 2

.... a molar amount of base was measured out to hydrolyze the bromosafrole, (which was obtained via
dmso/nabr/h2so4,in ~ 4 hours) to the secondary alcohol, which went smoothly, I think...the color changed from gold to greeny as soon as it was heated a little, heated a little more, driving off the methanol and most of the small amount of water present (there was a little used in dissolving the NaOH) but if I remember right, there was layer separation as the thing happened. This was done in a 125 ml glass funnel, returned the -ol to the flask, added dmso and a catalytic amount of base, which wasnt measured just a couple of dashes ....
upon heating the stuff changed to the exact color of performic ketone. The smell is not the same, but it definitely is no longer safrole, or the -ol, or bromosafrole....

It distills at exactly the same range as ketone, (20 deg below bromosafrole, and 20-25 above safroles) and is
pale yellow with a weird smell unlike anything in the batcave.

I believe I hear Master Bruce.........

*&^%$#
 
 
 
 
    element109
(Newbee)
06-09-00 12:58
No 15794
      Re: Alfred makes MDP2P via novel path?  Bookmark   

By any means post (or mail me) your results.
I'm thinking of giving the route a shot again.
I'm gonna write-up first what i'm going to do, show it to you guys, then i'm going to dream about it.


E109-