A novel and efficient method for the synthesis of substituted thiazepines and diazepines has been developed. A simple one-pot reaction of chalcones 1a–f with 1-amino-2-mercapto-5- phenyl-1, 3, 4-triazole and o-phenylenediamine in the presence of a catalytic amount of sodium acetate under microwave irradiation gave 2-(3, 8-diphenyl-7, 8-dihydro [1, 2, 4] triazolo [3, 4-b][1, 3, 4] thiadiazepin-6-yl) phenoles 2a–f and 2-(2-phenyl-2, 3-dihydro-1H-1 ...