A series of β-(trimethylsilyl)ethoxymethyl etherswere hydrolyzed to their corresponding alcohols in highyields by using a catalytic amount of CBr4 (15%) in MeOHunder refluxing reaction conditions. The chemoselectivedeprotection between trialkylsilyl and β-(trimethylsilyl)ethoxymethyl-protected alcohols can be achieved by usingan alcohol with steric hindrance such as iPrOH. Theselectivity also can be achieved in the CBr4/MeOH reactionmixture under ultrasonic reaction conditions.