The catalytic performance of mixed metal oxides was evaluated for the synthesis of diethylene glycol bis(allyl carbonate) (ADC) by transesterification of diethylene glycol (DEG), dimethyl carbonate (DMC). and allyl alcohol (AAH), and MgO-PbO was found to show the highest catalytic activity. The influence of preparation conditions on the catalytic performance of MgO-PbO was studied and its suitable preparation conditions were as follows. A calcination process was used, with Mg(OH)(2) and Pb(CH3COO)(2)center dot 3H(2)O as precursors, molar ratio of Mg:Pb = 6:1, and calcination temperature of 650 degrees C. Under the following reaction conditions, molar ratio of DEG:DMC:AAH = 0.08:1:2, weight percentage of MgO-PbO = 1.5% of total weight of all reactants, 100 degrees C, 6 h, and vacuum of 0.08 MPa, the yield of ADC was 97.3%. Moreover, MgO-PbO showed a good recyclability; ADC yield of 95.4% could be achieved after the catalyst was reused for two times. The results of N-2 adsorption-desorption measurement and XPS analyses for MgO-PbO indicate there exists an interaction between MgO and PbO, which promotes the catalytic performance and recyclability of MgO-PbO. Furthermore, the reaction pathway for ADC synthesis was elucidated by means of GC-MS analysis and experimental verification.