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