http://rhodium.lycaeum.org (http://rhodium.lycaeum.org)
Ill have to agree on that one .The reaction goes well.Then its a case of simple distillation
to remove the lower bp stuff.The next bit is where you succeed or stuff it.
Options are .1.Vacuum distill twice.2 Go to a proper frac distillation3 .Steam dist it out.
# 3 didnt work so well in this case, so its one or two.I didnt get a second chance, so im all ears on this one.
I used to steam distill. I would add several volumes of water (destroying all the acetic anhydride, but it was available in large quantities at the time) and then steam distill. I wouldn't acutally add any extra steam just raise the whole flask to boiling with a modified Dean-Stark trap and Friedrichs condenser fitted to the flask. The modified Dean-Stark trap I had added a glass tube from near the bottom of the collection tube to near the top of the reflow tube so that the water (which is heavier than the P2P) would flow back into the boiling flask and the P2P would collect in the trap. As the trap would fill with P2P I would open the stopcock to transfer it (and a small amount of water) to a sep. funnel.