Diphenylglycoluril was synthesized by condensation reaction of dibenzoyl from the oxidatetion of benzoin and urea. This study showed that with anhydrous ethanol used as solvent, sodium ethoxide as catalyst, the condensation reaction can be achieved at room temperature, the yield of product was higher , the average was 82% with the molar ratio of 2.5:1of urea and dibenzoyl, the dosage of catalyst 10% of dibenzoyl, 40℃，1.5h. The product was analyzed and characterized by IR、1H NMR、13C NMR and HPLC-MS. The results showed that the product structure was correct, and its pure was 98%. The method has the advantages of convenient operation, low reaction temperature, short reaction time, few catalysts and high yield and so on.