The essential idea of the work in this article is mainly dependent on the use ofbis‐hydrazonoyl halides for heterocyclic synthesis. The present work describes preparation and characterization of newbis‐thiazoles from reaction ofbis‐hydrazonoyl chlorides with thiosemicarbazones. The synthetic Schemes for the final compounds are proposed and discussed. Structures of the final products were elucidated by elemental analyses and Fourier transform infrared, mass spectrometry,1H, and13C‐NMR spectra.