Vibrating_Lights (Hive Bee)
09-06-01 08:50
No 210641
      Mdp2p from beta-nitroisosafrole  Bookmark   

Does any one have a link to a procedure to make mdp2p from beta-nitroisosafrole with acetic acid and iron.
 
 
 
 
    Osmium
(Stoni's sexual toy)
09-06-01 12:02
No 210687
      Re: Mdp2p from beta-nitroisosafrole  Bookmark   

PIHKAL. ../rhodium/
 
 
 
 
    Vibrating_Lights
(Hive Bee)
11-11-01 19:22
No 235555
      Re: Mdp2p from beta-nitroisosafrole  Bookmark   

What is electrolyctic iron.  what are the mechinisms involved in these reactions.
Shuligan reports an 80% yeild with this procedure add that with the 98+% isosafrole with KOH and the 74% in Nitrosaturation gives an Overall yeild of 54% ketone in respect to starting safrole.  Not to bad for OTC.
 
 
 
 
    Rhodium
(Chief Bee)
11-11-01 21:33
No 235581
      Re: Mdp2p from beta-nitroisosafrole  Bookmark   

It is iron powder, free of oxides.
 
 
 
 
    Vibrating_Lights
(Hive Bee)
11-11-01 22:48
No 235606
      Re: Mdp2p from beta-nitroisosafrole  Bookmark   

The Oxides can be removed with HgCl2 correct. would fine steel wool be suitable substitute for the iron powder taking into account the longer Rxn times.  RXN will procede until no iron is visible and reflux another 2Hrs. Then flood with water seperate and extract with DCM.  If the steel wool will work then swim likes the sound of this. 
Can anyone confirm yeilds of this type of a RXN.
VL_
 
 
 
 
    Osmium
(Stoni's sexual toy)
11-12-01 00:48
No 235652
      Re: Mdp2p from beta-nitroisosafrole  Bookmark   

You don't need any Hg in this reduction. The oxide won't harm your reaction since they will dissolve in the acid anyway.