The Vespiary

The Hive => Methods Discourse => Topic started by: Vibrating_Lights on September 06, 2001, 08:50:00 AM

Title: Mdp2p from beta-nitroisosafrole
Post by: Vibrating_Lights on September 06, 2001, 08:50:00 AM

Does any one have a link to a procedure to make mdp2p from beta-nitroisosafrole with acetic acid and iron.

Title: Re: Mdp2p from beta-nitroisosafrole
Post by: Osmium on September 06, 2001, 12:02:00 PM

PIHKAL.

https://www.thevespiary.org/rhodium/Rhodium/ (https://www.thevespiary.org/rhodium/Rhodium/)

Title: Re: Mdp2p from beta-nitroisosafrole
Post by: Vibrating_Lights on November 11, 2001, 07:22:00 PM

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.

Title: Re: Mdp2p from beta-nitroisosafrole
Post by: Rhodium on November 11, 2001, 09:33:00 PM

It is iron powder, free of oxides.

Title: Re: Mdp2p from beta-nitroisosafrole
Post by: Vibrating_Lights on November 11, 2001, 10:48:00 PM

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_

Title: Re: Mdp2p from beta-nitroisosafrole
Post by: Osmium on November 12, 2001, 12:48:00 AM

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