The aim of this study was to investigate effects of dehydrants on the trimethyl borate reaction and determine the kinetic parameters. Thus, trimethyl borate was produced by reacting of boric acid with methyl alcohol in a rotary evaporator. Evaporator was programmed to operate at 65 degrees C temperature and 150 rpm. Formed water at this reaction affects the reaction rate and trimethyl borate formation, negatively. Therefore, water is necessary to be removed from the reaction media. Kinetic search of the process gives reaction rate and rate constant as, pseudo first order and 0.0613 min(-1), respectively. Consequently, the rate equation can be mentioned as r=0,0613 C-B(OCH3)3. Since the capacity and intensity properties changed with dehydrant type, various dehydrants at different amounts should be tested in the reaction. For this purpose CaCl2 and LiCl were used as dehydrant in the reactor, separately. During the reaction, trimethyl borate was distilled in the form of an azeotrope with methanol. LiCl salt was also used to separate azeotrope into two layers. Top layer was rectified and determined as trimethyl borate compound by using GC-MS instrument. In addition, purity of trimethyl borate was determined by titrimetric method.