Chem. Abstr., 109, 92296:
Nitriles of b.p. 150 were prepd. by dehydration of amides with POCl3 in a mixed solvent of N,N-di-substituted anilines or N-substituted anilines and
halohydrocarbons or arom. hydrocarbons followed by simple distn. of the resulting reaction mixt. Thus, POCl3 was added dropwise to suspension contg.
ClCH2CONH2 in C6H6/PhNMe2 at 60 over 5 h, the reaction mixt. was kept for 2 h, and then subjected to simple distn. at 100 under 40 torr. The obtained
distillate was rinsed with aq. NaOH and subjected to rectification to give 71% ClCH2CN, vs. 50% for reaction mixt. which was neutralized at pH 8
before rectification. |