The electrochemical oxidation of catechol has been studied in the presence ofp-nitroaniline as a nucleophile in aqueous media at the surface of glassy carbon electrode, using cyclic voltammetry. The products of electrosynthesis have been purified and characterized by Fourier-transform infrared (FT-IR), 1H nuclear magnetic resonance (NMR), 13C NMR, and distortionless enhancement by polarization transfer (DEPT), and the mechanism of anodic oxidation was deduced from voltammetric and spectroscopic data.