Abstract: This paper reports the synthesis of a new nitrogen-containing crown ether compounds (azacrown-ether). Condensation of 1, 2-bis(ω-chloro-polyoxaalkyl)-benzene such as 1, 2-bis (5-chloro-3-oxa-l-pentyloxy)-ben-zene, 1, 2-bis(8-chloro-3, 6-dioxa-l-octyloxy)-benzene and 1,2-bis (11-chloro-3,6,9-trioxa-1-undecyloxy)-benzene with N, N′, N"-tritosyl diethylenetriamine or N, N′, N", N′"-tetratosyl triethylenetetraamine disodium salts in anhydrous DMFat reflux temperature for 7-8 hours produced six new nitrogen-containing crown ether compounds, yield 46-75%.