This study is concerned with the cathodic reduction of 4-nitroso-N,N-dimethylaniline to 4-amino-N,N-dimethylaniline in 1.0 M HCl and 1.0 M H2SO4 containing 10% MeOH. The effect of cathode material, supporting electrolyte, electroactive compound concentration, temperature and current density in the electrochemical synthesis of 4-amino-N,N-dimethylaniline were investigated. The best cathode material was tin, which gave a selectivity of 92.7% with a current yield of 90.3% at a current density of 6 mA cm(-2). The final electrolysis product was obtained as its respective HCl and H2SO4 salts and their structures were elucidated using spectrochemical techniques.