Poodle (Stranger)
03-29-01 00:09
No 180749
      Simplifying P2P from bzcl and acetonitrille  Bookmark   

In a dream, 0.2 mol benzylmagesiumchloride grignard reagent were prepared by standard methods in diethylether (Total reaction volume: 200ml). Reaction intitated by heating the mixture to 60 degrees for a short periode of time. About 2 moles of acetonitrille (100ml) was mixed with 100 ml of waterfree diethylether and cooled in ice/water. The benzylmagnesiumchloride solution was added the acetonitrille over a periode of 10 minutes, using constant swirling of the reaction mixture. A white percipitate was formed, corresponding to a intermediate complex, not soluble in ether or acetonitrille. This complex was isolated by filtration through a buchner, and washed twice with water-free ether to remove any unwanted remains of acetonitrille or Bzcl. The white complex was briefly dried, but as it began to turn yellow, no chances was taken and 15 ml destilled water was added, then another 10 ml (The complex reacted immediatly with the water, giving heat and causing remaining ether to boil, the solution turned yellow/orange with oily orange bubbles.) The solution was exposed for a vaccum to remove any remaining ether in the solution. Upon using the vaccum, ether was removed and the solution separated into two layers with an orange oil on top and a water layer containing salts and unsolved salts. The oily layer was separated and gave 21 ml of possible P2P, about 75-80% of the theoretical 26 ml. The ketone was frozen at -20, responding to that temperature by forming a solid, as theoretically expected by a substance having a melting point at -16.

This method could be of interest for producing P2P from acetonitrille, as it greatly simplifies the procedure by eliminating any need for extensive extraction of the ketone.


Ref:Jerry March. 4th. Ed.,page 935-936

"The above is just a result of a confused mind, do not try this at home kids !"

(Hive Addict)
04-03-01 07:45
No 181761
      Re: Simplifying P2P from bzcl and acetonitrille  Bookmark   

It would be interesting to further verify that you have P2P, say by preparing the bisulfite addition compound.