Disulfides play important roles in biological and chemical processes. Oxidation of thiols is the most exploited method for disulfide synthesis. Trichloromonoxomolybdenum (V) has been found to be a superior oxotransfer reaction catalyst for the conversion of thiols to the corresponding disulfides in excellent yields under mild reaction conditions. A viable kilo-scale synthesis of the symmetrical disulfide was described. Simple workups, economical and practical are the some advantages of this method.