An improved process for preparing dihydrocarbyl substituted dithiocarbamates of molybdenum wherein an alkali metal hydroxide is reacted with a mixture of a dihydrocarbyl substituted amine and carbon disulfide in an aqueous solution to produce an alkali metal salt of dithiocarbamate and the alkali metal salt then reacted with an alkali metal molybdate in the presence of acid to produce the dihydrocarbyl substituted dithiocarbamate of molybdenum. The process is completed in an inert atmosphere and within a relatively narrow range of temperatures so as to avoid the production of by-products which have heretofore reduced both the yield and purity of the final product. The preparation of the alkali metal salt of dithiocarbamate is completed at a temperature generally within the range from about -5 to about 30.degree. C. The acidification of the alkali metal salt of dithiocarbamate is completed, generally, at a temperature within the range from about -5 to about 5.degree. C.