The present study pertains to the photochemical oxidation of p-chloroaniline using TiO2 (catalyst) and H2O2 (oxidant) obtained the corresponding 4,4- dichloroazobenzene (I), 4,4-dichloroazoxybenzene (III) and an unexpected 4,4- dichloro-2-hydroxyazobenzene (II) was also formed in low yield due to the photochemical Wallach rearrangement of the 4,4-dicholoroazoxybenzene. Almost 84% of 4,4-dichloro azoxybenzene derivative was obtained when using TiO2 along with H2O2. Then, with a mixture of HY-zeolite and TiO2 along with H2O2 in which the percentage of compound I was increased (79%) with the...