The oxidation of cyclohexylamine (CHA) was carried out in a batch reactor, using Fenton’s reagent. The effects of the following parameters were investigated: residence time, pH level, ferrous ion concentration, and hydrogen peroxide concentration. Residence time ranged from 30 min to 2 h, and its effect was found to be significantly positive. A pH of 3 for the medium was observed to be optimum. Ferrous ion and hydrogen peroxide concentrations ranged from 0.1 g/l to 0.265 g/l and from 0.5 g/l to 1.3 g/l, respectively. The influence of hydrogen peroxide was significant at 0.16 g/l of ferrous ions and a pH of 3. CHA removal efficiency was measured by calculating chemical oxygen demand (COD). The maximum COD removal efficiency was 62%, and the minimum yield of ammonia was 14%. The yields of nitrite and nitrate were negligible. Overall, the results proved the effectiveness of the Fenton process for the treatment of CHA.