Schiff’s bases has been synthesized by bulk electrochemical method from 5-amino-2-hydroxy benzaldehde and salicylaldehyde. The product was characterized by spectroscopic techniques. It involves the electrochemical reduction of 5-nitro-2-hydroxy benzaldehyde. The electrochemical reaction has been carried out at copper and silver electrodes in the presence of sodium chloride as supporting electrolyte in water/methanol (50 : 50) solution. The electrochemical reaction has also been performed in presence of sodium sulphate as supporting electrolyte. The electrochemical behaviour of the product was investigated in aqueous methanolic solution at different time interval. The electrochemical reaction has been carried out at copper cathode and silver anode. The electrochemical synthesis was carried at the cell voltage of 30 V and highest current density required for the reduction of nitro group has been achieved.