Recently the synthesis of 4-dimethylaminobenzoinhydrazone were carried out by the condensation of 4-dimethylaminobenzoin with hydrazine hydrate in presence of aqueous sodium hydroxide in Dioxane-water (80%) medium respectively. Similarly 4,4'-dimethoxy benzoin hydrazone were synthesized by the interaction of 4,4'-dimethoxy benzoin with hydrazine hydrate in presence of aqueous sodium hydroxide in dioxane-water (80%) medium respectively. The synthesis of 4-dimethylaminobenzoin and 4,4'-dimethoxybenzoin were carried out by the known literature method. The structure of all the synthesized compounds were justified on the basis of chemical characteristics, elemental and I.R. and NMR spectral analysis.