Objectives:The aim of this study was to synthesize, characterize, and screen some new 1-(4-((2-(4-substitutedphenyl)hydrazono)methyl)phenyl)-1H-1,2,4-triazole derivatives for their antimycobacterial activities.Materials and Methods:The target compounds (2a-h) were gained by condensation of 4-(1H-1,2,4-triazol-1-yl)benzaldehyde with appropriate phenylhydrazines. Their structures were elucidated by IR, 1H-NMR, and mass spectrometry. The antimycobacterial activities of the compounds were determined in vitro against Mycobacterium tuberculosis H37Rv.Results:The biological assay results showed that the methylsulfonyl-substituted derivative 2f displayed the highest antimycobacterial activity in this series.Conclusion:Although the methylsulfonyl-substituted derivative exhibited significant antimycobacterial activity, none of the synthesized compounds was as effective as isoniazid, rifampin, ethambutol, and ciprofloxacin against M. tuberculosis.