Electrochemical oxidation of Naphthalene-2,3-diol (1) has been studied in aqueous and nonaqueous solution by the use of cyclic voltammetry, differential pulse voltammetry and chronoamprometry. Recorded cyclic voltammograms (CVs) at various pHs (pH=1-8) show that 1 oxidized to its corresponding o-benzoquinone derivative (1ox) and the electrode reaction is a two-electron, two-proton process (1,2). Irreversible CVs indicates that produced o-benzoquinone (1ox) is unstable and participates to a following chemical reaction. The effect of different parameters such as pH, Naphthalene-2,3-diol (1) concentration and time window of chosen electrochemical method on the following chemical reaction has been discussed. In order to prove of two-electron, two-proton both electrochemical and computational study were performed (3). Also the value of diffusion coefficient of 1 was determined by the use of Cottrell plots by chronoamperometry.