Trimethylsilylation of a variety of alcohols and phenols, in the presence of silica chloride, using hexamethyldisilazane (HMDS) in solution and under solvent-free conditions is reported. Trimethylsilyl ethers were formed in excellent yields both for aliphatic alcohols and phenols without having an electron-withdrawing group. In addition, SiO2-Cl can be recovered and reused after drying.