Polymer-anchored azo complexes of Cu(II) and Ni(II) were synthesized by the reaction of chloromethylated polystyrene, 3-aminophenol, and 1-nitroso-2-naphthol with the metal chlorides. The catalytic activities of these complexes were studied in the oxidation of various organic substrates including alkenes, alcohols, alkanes, and sulfides with 30 % aqueous hydrogen peroxide. The structures of both catalysts have been investigated by physiochemical methods. Both catalysts proved to be very stable and could be reused more than five times without significant loss of activity. Furthermore, these catalysts require very mild reaction conditions.