Cetyltrimethylammonium peroxodisulfate (CTA)2S2O8 was quantitatively prepared and used for the oxidation and deprotection of trimethylsilylethers to the corresponding carbonyl compounds in acetonitrile. Selective oxidation of allylic or benzylic trimethylsilylethers in the presence of saturated alkyltrimethylsilylethers were also achieved. This new reagent is more efficient and has several advantages over