In this study, the diazonium salts of 4-amino-3,5-dimethyl-1H-pyrazole (1A), 5-(4-aminophenyl)- 3H-1,3,4-oxadiazoline-2-thione (1B), 5-(4-aminophenyl)-2,4-dihydro-4-cyclohexyl-3H-1,2,4-triazole-3-thione 1(C), 5-(4-aminophenyl)-2,4-dihydro-4-phenethyl-3H-1,2,4-triazole-3-thione 1(D) and 5-(4-aminophenyl)-2,4-dihydro-4-phenyl-3H-1,2,4-triazole-3-thione (1E) which were previously prepared by us, were coupled with acetylacetone. The structure of the substances were elucidated using elementary analysis and uv, ir, ¹H nmr, ¹³C nmr, mass spectral data. These spectral data showed that the coupling products were in hydrazon form. Keywords :