Department of Chemistry, Mahatma Gandhi Campus, Bhavnagar University, Bhavnagar-364 022, Gujarat, India E-mail : drgodhani@yahoo.com Manuscript received 02 November 2()10, revised 14 September 2011, accepted 08 November 2011 4-Nitro benzoyl isothiocyanate (1) is prepared by a reaction of 4-nitro benzoyl chloride and ammonium isothiocyanate. Compound 1 reacts with phenyl hydrazine in the presence of acetone to form 5-(4-nitrophenyl)-l-phenyi-1H-1,2,4-triazole-3(2H)-thione (2). Compounds 2 on reaction with formaldehyde and different aromatic amines in 1,4- dioxane yielded 2-(substituted-amino)methyl-5-(4-nitrophenyl)-1-phenyl-1H-1 ,2,4-triazole-3(2H)-thione (3a-j) respectively. The synthesized compound 3a-j were screened for their antibacterial and antifungal activities and characterized by spectral techniques like IR and NMR.