In this study, new azopyrazole substituted 2,4-dihidro-3H-1,2,4-triazole-3-thione and 2,3-dihidro-2-ethylimino-1,3,4-thiadiazole were synthesized using 1-phenyl-3,5-dimethyl-4-(p-hidrazinocarbonilphenylazo) pyrazole as a starting material. Furthermore, the azo groups of substances were reduced with hydrazine hydrate. The structure of these substances were elucidated using UV, IR, NMR (for substance 2, 3 and 4) and Mass (for substances 3 and 4) spectral methods besides elementary analysis. Keywords :