M-xylylene diisocyanate (XDI) is an important special isocyanate that draws more and more attention in recent years. The introduction of the –CH2– group between the benzene ring and isocyanate group, which makes it resistant to yellowing, can be applied in the fields of high value-added polyurethanes, such as high-grade coatings, medical polyurethane, high-grade optical polyurethane, and so on. M-xylylene dicarbamate (XDC) is the key intermediate for the synthesis of XDI via the non-phosgene thermal decomposition route. In this work, a novel methodology for the synthesis of XDC via carbonylation of m-xylylenediamine (XDA) using urea as carbonylation reagent over TiO2 catalyst was proposed. The standard XDC sample was first synthesized by the reverse reaction between XDI and ethanol, and then, the qualitative analysis of the standard XDC sample was characterized by FT-IR and 1H-NMR to confirm its structure. The standard curve of XDC was then successfully established in liquid chromatography with a correlation coefficient of more than 0.999. The qualitative analysis of the target product was carried out by GC-MS, and the reaction path was primarily speculated. Furthermore, the effects of different catalysts, reaction temperature, reaction time, the molar ratio of raw materials, and catalyst dosage on the yield of XDC were studied. The results showed that using TiO2 as the catalyst, under the optimized conditions, the reaction temperature of 205℃, the reaction time of 6 h, n(urea):n(XDA) of 3:1, the amount of catalyst was 15wt% XDA, the conversion of XDA was 100%, and the yield of XDC could reach to as high as 82.4%. Therefore, this process not only provides a feasible route for green, effective, and economic production of XDC, but also provides a theoretical basis for the non-phosgene synthesis of special isocyanate XDI.