A series of novel p-toluenesulfonyl-hydrazinothiazoles and hydrazino-bis-thiazoles derivatives (2a-f, 3a-f and 5-8) were synthesized by initial condensation of p-toluenesulfonylthiosemicarbazide 1 with a series of α-halogenocarbonyls in acetone or dimethylformamide (DMF)/acetone, mixture. All our synthesized compounds were submitted for further acylation reaction in the presence of acetic anhydride. The structures of newly synthesized derivatives 2a-f, 3a-f and 5-8 were confirmed by IR, (1)H-NMR, EIMS spectral data and elemental analysis. Compounds 2a, 2c, 2d, 2e and 3a showed significant anticancer activities (IC(50)<10 μM) on both prostate DU-145 and hepatocarcinoma Hep-G2 cancer cell lines.