Chemoselective preparation of O-acylated derivatives from bis-protected mercapto alcohols was described. Trialkylsilyl and trialkylstannyl chloride are used to generate an intermediate with O-and S-protection. The intermediates from β-mercapto alcohols are reactive toward acylating agents and selective to provide O-acylated derivatives. The present preparation involves the direct conversion of alcohol to the corresponding O-acylated compounds ...