In this study, zinc acetate was used as catalyst for the synthesis of dimethyl carbonate (DMC) through the reaction between methyl carbamate (MC) and methanol (urea alcoholysis process). The effect of the temperature on the DMC yield was investigated in batch catalytic mode. It was uncovered that the DMC yield increased with increasing the temperature; however, the moderate temperature (165 °C) was selected as the optimal temperature because the undesired byproduct (NMMC) was at the lowest level while the DMC production yield remained also high enough.