A highly selective cleavage of MEM ethers has been achieved in high yields using CeCl<SUB>3</SUB>·7H<SUB>2</SUB>O in refluxing acetonitrile under mild and neutral reaction conditions. The method is very rapid and compatible with other hydroxyl protecting groups such as Bn, TBDPS, Ac, Me, Tr, PMB, benzylidene, THP, MOM, BOM, and NHAc present in the substrate