A series of substituted 1, 2, 4-triazole derivatives have been synthesized, using chloroform mediated phenylimino dichloromethane. It was added to a chloroform suspension of N'-(arylidene) ethanehydrazonohydrazide and the mixture was refluxed over water bath for 3 hours. The evolution of hydrogen chloride gas was noticed. The structures of synthesized compounds are confirmed on spectral analysis like IR; 1H NMR and 13C NMR data. All newly synthesized compounds were screened for their antimicrobial activity towards Gram-positive and Gram-negative bacterial strains and antifungal activity including  B. subtilis, E. coli, S. aureus, S. ablong, Candida and A. niger. Results showed that most of compounds have measurable antibacterial and antifungal activity.