Three new [3+3] polyazamacrocycles were prepared by a one-step reaction with isophthaloyl chloride, di(4-aminophenyl)methane, di(4-aminophenyl)ether and di(4-aminophenyl)sulfone as the starting materials in the yields of 41%, 40% and 36% respectively; The structures of products were characterized by elemental analysis, IR ,1H NMR, 13C NMR and MALDI-MS techniques.