A novel series of 2-(3-aryltriaz-2-enyl)acetonitrile (5a-j) have been synthesized by using aminoacetonitrile hydrogen sulfate. The synthesized compounds were evaluated for their antibacterial activity against two gram positive bacteria (Staphylococcus aureus, Bacillus subtilis), two gram negative bacteria (Escherichia coli, Pseudomonas aeruginosa) and antifungal activity against one fungi (Candida albicans). The structures of the newly synthesized compounds have been elucidated on the basis of IR, 1H NMR, MASS Spectral data and elemental analysis.