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A series of new 2-(phenylthio) benzoylarylhydrazones were synthesized by acid-catalyzed condensation of hydrazide 3 with corresponding aldehydes. The chemical structures of the compounds were elucidated by FT-IR, 1 H-NMR and Mass spectra. All newly synthesized compounds were evaluated for their antimycobacterial activities against Mycobacterium tuberculosis H 37 Rv using the microplatealamar blue assay (MABA). Compounds 4f (5-Nitro-2-furyl analogue) and 4g (5-Nitro-2-thienyl analogue) showed antimycobacterial activity with IC 90, 7.57 and 2.96 μg/mL, respectively.