MgO/ZrO2 catalyst was prepared for the synthesis of 1,6-dicarbarnate hexane (HDC) using dimethyl carbonate (DMC) and 1,6-diamine hexane (HDA) as raw materials. When the catalyst is calcined at 600 degrees C and MgO load is 6 wt%, the catalyst exhibits better activity. When the concentration of catalyst is 2 g (100mL)(-1) DMC, n(HDA):n(DMC) = 1: 10, reaction time is 6 h under reflux temperature, and the yield of 1,6-dicarbarnate hexane is S3.1%. HDC yield decreases from 53.1% to 35.3% after MgO/ZrO2 being used for three times. The decrease in specific surface area may be attributed to deactivation of MgO/ZrO2.