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New series of substituted thiazole were prepared starting from thiosemicarbazone derivatives 1a,b by reacting with different reagents namely, hydrazonoyl chlorides, dimethyl acetylene dicarboxylate, phenacyl bromide, chloroacetone, and chloroacetic acid. The structures of the newly synthesized compounds were elucidated on the basis of elemental analyses and spectral data. Some representative examples of the newly synthesized compounds were screened as antitumor agents against all the 60 cell lines of the NCI-60 cell panels. The tested compounds were active only against MCF7, SF268, SF295, HT29, HT29, COLO205, COLO205, K562, HL60, A549-ATCC, H460, LOXIMVI, OVCAR3, OVCAR4, OVCAR5, OVCAR8, SKOV3, PC39, DU145 and A498 while inactive against other cell lines in the panel.