Organic compounds with a nitrogen-containing functional group play an exceptional role in natural and technological processes. In particular, such compounds are highly useful for medicinal purposes, dyes, pesticides, explosives, etc. The great theoretical and practical importance of these compounds has stimulated the study of the chemical properties of nitrogen-containing functional groups. Among organic nitrogen compounds, Azoxybenzenes (AZB) occupy a special place. As a result of their high thermal and chemical stabilities, all the compounds containing a nitrogen atom attached to the benzene ring can be ultimately converted into AZBs via oxidation or reduction reactions [1]. AZBs are widely applied in pharmaceuticals, oxidants, polymer inhibitors, and stabilizers. In light of their importance, the development of AZB derivatives has become a hot topic for a long time. Therefore according to the mentioned features, the electrochemical behavior of AZB at a glassy carbon electrode in the different aqueous buffered solutions was studied via cyclic voltammetry (CV), chronoamperometry, and chronopotentiometry techniques. The CV of AZB showed that azoxybenzene undergoes an irreversible 4e/4H+ reduction reaction and converts to Hydrazobenzene (HYB), which then undergoes a reversible 2e/2H+ oxidation reaction to generate azobenzene [2]. In this regard, Differential pulse voltammetry (DPV) was used to determine the number of transferred electrons. For more data, the diffusion coefficient of AZB was obtained using the chronoamperometry method. In the last decades, electrosynthesis has been known as a green and powerful tool for developing environmentally friendly synthetic processes [3]. In this work, we have also synthesized the new AZB derivative by reduction of AZB in the presence of Benzenesulfinic acid (BSA) in an aqueous buffered solution (pH = 2.0, C = 0.2 M H3PO4) via the controlled potential electrolysis (-0.78 V vs. Ag/AgCl electrode) under green conditions and with
