The oxidation of alcohols to carbonyl compounds was studied using potassium hexacyanoferrate(III) mediated by nitroxyl radical as the catalyst under polymer-supported organic–aqueous two-phaseconditions. Primaryalcohols are readily oxidized to the corresponding aldehydes in excellent yield with no over-oxidation to carboxylicacids. Secondaryalcohols are converted to the corresponding ketones with