The hydrazono derivatives 3 and 4 have been synthesized by the reaction of diazonium salt of 4-(phenyldiazenyl)-aniline 1 with active methylene compounds, ethyl acetoacetate and diethyl malonate respectively. 2-[4'-(Phenyldiazenyl)-phenyl]-hydrazono-N-heterocyclic compounds (5-6) & (7-8) were obtained from ethyl-3-oxo-2-{2'-[4 ''(phenyldiazenyl)-phenyl]-hydrazono}-butanoate 3 and diethyl-2-{2'-[4 ''-(phenyldiazenyl)phenyl]-hydrazono}-malonate 4 respectively. Structural assignments were based on elemental analysis & spectroscopic data (IR, (1)H NMR).