O-Anisidines (OAs) are extensively used as an intermediate for chemical reactions to produce various triphenylmethane and azo dyes, and also in manufacturing numerous pigments. They are found to be highly toxic and have carcinogenic properties, so it is imperative to treat OA solutions before disposal. In this study a promising approach to degrade OA solutions has been carried out using Fenton’s reagent. Oxidation trials were conducted for 24 hours and various parameters – OA removal, pH, effect of H2O2 and Fe2+, and COD removal – were analysed to understand the oxidative degradation of OA. For varying initial OA concentrations, the OA and COD removal efficiencies of 72 to 85% and 62 to 74%, respectively, were obtained at pH = 3, and at different optimum H2O2 and Fe2+ doses. Lower initial concentrations of OA showed better removal efficiencies. The reaction time was estimated to 360 minutes after which there was negligible degradation occurs.