Dimethyl toluene-2,4-dicarbamate (TDC) is an important intermediate for the nonphosgene manufacture of toluenediisocyanate. The synthesis of TDC from 2,4-diaminotoluene (TDA), urea, and methanol is a green route with a good industrialization prospect. So, the study on its reaction kinetics is of great significance. First, the reaction network was structured and simplified on the basis of experimental result analyses. Second, the experimental data for kinetics were measured on an autoclave. Last, the reaction kinetics model was established by means of parametric estimation. Model test results showed that the prediction values of the reaction kinetics model agreed well with the experimental data Therefore, the reaction kinetics model can be used in the process analyses and scale-up of the reaction of TDA, urea, and methanol to TDC.