反应详情

A 100 ml three-necked round bottom flask equipped with a dry ice condenser, magnetic stirrer, gas inlet and thermometer was charged with 40 ml of diethoxymethane, 5.0 g of ethyl 3-ethoxypropionate and 1.00 g dodecane (an internal standard for gas-liquid chromatography analysis), and the flask was placed in a 30° C. water bath. Ketene gas, produced by cracking diketene in a 550° C. furnace, was added until the solution became saturated. A portion (0.1143 g) of the catalyst prepared as described above and stored for one week at room temperature, was added on the tip of the thermometer. An exothermic reaction ensued, briefly raising the pot temperature to 80° C. The mixture was kept saturated with ketene for 30 minutes. The mixture was then analyzed by gas-liquid chromatography, and it was found that the 0.1143 g of catalyst had produced 17.3 g of ethyl 3-ethoxypropionate, not including the 5 grams added at the start. This catalyst was thus capable of producing 156 g of ethyl 3-ethoxypropionate for each gram of catalyst.

1. customA 100 ml three-necked round bottom flask equipped with a dry ice condenser, magnetic stirrer, gas inlet
2. customwas placed in a 30° C.