A simple and efficient catalytic oxidation of urazoles and a bis-urazole to the corresponding triazolinediones by treatment with Al(NO(3))(3)center dot 9H(2)O in the presence of a catalytic amount of silica sulfuric acid is described. A good range of urazole derivatives was selectively oxidized in CH(2)Cl(2) at room temperature in good to excellent yields.