A semicontinuous process for the synthesis of methyl carbamate from urea and methanol was investigated in the autoclave without the catalyst. Some significant parameters were determined in terms of the methyl carbamate yield. The optimal reaction conditions were found at an initial molar ratio of methanol/urea of 6:1, a reaction temperature of 423 K, a flow rate of fresh methanol at 4 mL/min, a stirring speed of 800 rpm and a reaction time of 6 hours, respectively. A MC yield of 98.7% was obtained at the optimal reaction conditions. Furthermore, the kinetics of this reaction were researched and the reaction activation energy was obtained as 110.498 kJ/mol. It was demonstrated that removing methanol containing ammonia from the autoclave and replacing it with continuously feeding fresh methanol resulted in a higher reaction rate and a high MC yield.