Electro-organic Synthesis of 3,3'-bis( hydroxymethyl)hydrazobenzene has been carried out by the electro reduction of m-nitrobenzaldehyde has been studied at copper and amalgamated forms of copper and zinc electrodes under alkaline conditions using galvanostatic techniques. Isolated product was characterized by T.L.C., usual laboratory qualitative tests and IR, NMR spectral analysis to be 3,3'-bis (hydroxymethyl) hydrazobenzene. Effect of different parameters like current density, temperature, depolarizer concentration and nature of cathode material on yield percentage and current efficiency have been investigated. Number of electrons have also been calculated to confirm the isolated product to be 3,3'-bis(hydroxymethyl) hydrazobenzene.