The methoxycarbonylation of 2,4-toulene diamine and 4,4'-diphenylmethane diamine with dimethyl carbonate to the corresponding dicarbamates using zinc acetate was carried out at 453 K. Zn(OAc)(2), prepared by evacuating Zn(OAc)(2).2H(2)O at 383 K for 2 h, yields dimethyltoulene-2,4-dicarbamate in 96% yield in 2 h, while Zn(OAc)(2).2H(2)O yields dimethyl-4,4'-methylenediphenyldicarbamate in 98% yield at 453 K in 2 h. The structure of methyl 3-amino-4-methyl phenyl carbamate, which is one of the intermediates for the reaction of 2,4-toulene diamine with dimethyl carbonate into dimethyltoulene-2,4-dicarbamate, has been determined by measuring the NOE spectrum of H-1 NMR.