Przemysl Chemiczny, Vol.85, No.8-9, 584-586, 2006
Studies on improving the process yield and purity of o-ethoxyhenzamide
A (0.2:0.3:0.3:0.025 by moles) salicylamide-EtCl-K2CO3-Kl mixt. was heated in 50 ml acetone to 100 degrees C within 1 hr. and then 10 hrs. at 100 degrees C/0.3-0.4 MPa to yield o-ethoxybenzamide in 85.4% yield. The reaction mixt. was poured onto water and the amide collected by filtration with I g C or the acetone was distd. off. The resulting 99.93% pure amide contained salicylamide 0.03 and unidentified (HPLC) impurities 0.04%. The conventional process run in aq. EtOH gave the amide in 65-66.7% yield with <= 0.5% of impurities.