Organo-nitrogen compounds play an important role in the industrial and biological chemistry. Photo-assisted oxidation of p-anisidine by Fenton reagent has been studied. The effect of different reaction parameters such as concentration of substrate, H2O2, FeSO4, pH and polarity of solvent were studied. The progress of the reaction was observed by TLC. Photoproduct was characterized by physical, chemical and spectral methods. A tentative mechanism has been proposed for overall reaction.