Recently, the synthesis of 2-hydroxybenzoinoxime, 2-hydroxy-benzoinhydrazone, 2-hydroxybenzoinphenylhydrazone and 2-hydroxybenzoin-semicarbazone with hydroxylamine hydrochloride, hydrazine hydrate, phenyl hydrazine and semicarbazide hydrochloride in presence of aqueous sodium hydroxide in DMF-water (80%) medium respectively. Similarly, furoinoxime, furoinhydrazone, furoinphenylhydrazone, furoinsemicarbazone were synthesized by the interactions of furoinbenzoin with hydroxylamine hydrochloride, hydrazine hydrate, phenyl hydrazine and semicarbazide hydrochloride in presence of aqueous sodium hydroxide in DMF-water (80%) medium respectively. The synthesis of 2-hydroxybenzoin and furoinbenzoin 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.