Abstract An efficient and convenient procedure for the trimethylsilylation of a wide variety of alcohols, including primary, benzylic, secondary, and phenols with hexamethyldisilazane, has been developed. The reactions were carried out at room temperature in the presence of a catalytic amount of niobium (V) chloride and afforded the corresponding trimethylsilyl ethers in high to excellent yields in short time. GRAPHICAL ABSTRACT