A simple and efficient method has been developed for the hydrolysis of methoxymethyl (MOM) ethers and esters to the corresponding alcohols and acids employing a catalytic amount of bismuth triflate in an aqueous medium. The conversions occur at ambient temperature and the yields of the deprotected alcohols are very good. The reaction was highly selective in the presence of other protecting groups such as TBDMS, TBDPS, benzyl, and allyl ethers.