300.0 g of methyl acetate and 16.5 g of sodium methoxide were added to a high-pressure reactor. CO gas was then introduced to a pressure of 3.0 MPa. The reaction temperature was maintained at 60 °C, and the CO pressure was controlled at 3.0 MPa. After the reaction was complete, the solution was transferred to a distillation vessel to remove excess methyl acetate. 131.4 g of a 10% hydrogen chloride methanol solution was slowly added dropwise at a reaction temperature of 65 °C. After post-treatment, concentration, and distillation, 30.6 g of methyl 3,3-dimethoxypropionate was obtained, with a purity of 95.7% and a yield of 66.2%.