As the thiazolyl group has great importance as it appears frequently in the structure of various natural products, biologically active compounds and in some antibiotic drugs, a series seven thiazolyl hydrazone derivatives have been synthesized from substituted aromatic ketones, thiosemicarbazide & α-halo ketones via one-pot approach with good yields. All the synthesized compounds were characterized by IR, 1H NMR, 13C NMR and Mass Spectroscopy. In the future, the synthesized thiazolyl hydrazones would lead the promising pharmacological properties. Hence, there is enough scope to explore new compounds incorporating substituted thiazolyl moiety, which would lead to the development of novel derivatives with potential activity.