Abstract An efficient procedure for the trimethylsilylation of alcohols and phenols is presented. The combination of 1,1,1,3,3,3-hexamethyldisilazane and a catalytic amount of phenyltrimethylammonium tribromide (PhMe3N+Br3 −) was found to be effective for the trimethylsilylation of alcohols and phenols. The protection reaction is very simple and homogenously performed in dichloromethane at room temperature and mild conditions.