C–H oxidation of anthracene and eight other alkylarenes with binuclear macrocyclic complex of CoIII–CuII as a catalyst in the presence of 30% aqueous hydrogen peroxide to the corresponding carbonyl compounds were studied. The oxidation took place selectively at the benzylic C–H bond and no oxidation was observed in aromatic ring. The reaction is simple, clean and high yielding and generates water as the only by-product.