The catalytic activities of first row transition metal oxides in the conversion of p-nitrophenol to p-aminophenol were investigated. The conversion was carried out at room temperature (30° C) using aqueous sodium borohydride. The reduction process was accelerated by CuO, Co3O4, Fe2O3 and NiO. The oxides such as TiO2, V2O5, Cr2O3, MnO2 and ZnO were found to be inactive towards the conversion of the nitrophenol. The active catalysts were analyzed before and after the reaction by XRD and the reduction reaction was monitored and confirmed by UV–vis, HPLC, 1H NMR and FT-IR techniques.