Diester compounds are widely used in the fields of organic intermediates, drugs, plasticizers, spices and so on. In this paper, we reported that the deep eutectic solvent (DESs) catalyzed esterification of dicarboxylic acids with alcohol to synthesize diester compounds. The maximum yield of diester compound was up to 95%. After the catalyst was recycled for 8 times, the yield of the product is still over 88%. All products were characterized by 1H NMR and 13C NMR. This method has the advantages such as simple operation, high yield, easy separation and catalyst recycling.