In this work 1,2,4-Triazole and 1,3,4-Oxadiazole derivatives were synthesized from [4-(4-hydroxy-3-methyl naphthyl) diazenyl] benzoic acid [M1], which were converted to [4-(4-hydroxy-3-methyl naphthyl)diazenyl] benzoate [M2]. Benzoate derivative reacted with hydrazine afforded [M3] which cyclized by carbon disulfide to give compound [M4]. In addition, cyclization of compound [M3] was accomplished by sodium hydroxide and thiosemicarbazide to give triazole- thiol [M5]. Hybrid polymers [M6 and M7] were synthesized by grafted 1,3,4-oxadiazole [M4], and 1,2,4-triazole [M5] onto the polyvinyl chloride in the presence of pyridine and tetrahydrofuran. These compounds were characterized by the following techniques: FT-IR, and 1H, 13C NMR spectroscopies, and elemental analysis C,H,N,S. The biological activity study, IC50 value was significantly decreased in M6 (IC50=25.76 µM/ml) and M7 (IC50=21.41 µM/ml). In addition, the biological activity for final products achieved with good results.