Synthesis
In a 250m1 round bottom flask, 5g of sodium carbonate, 10g of cobalt octacarbonyl, 72ml (57g, 1. 25mol) of ethanol and 53ml (61g, 0. 5mol) of ethyl chloroacetate were added, and CO2 was passed through the gas at a flow rate of 50m1/min for 6h, and the reaction was completed. To the system was added 5 m1 of concentrated sulfuric acid, shaken for 15 min, and then distilled under reduced pressure to collect the 80C/4 mmHg fraction. Add 60ml of water to the distillate, adjust the pH to 0.3 with concentrated sulfuric acid, vibrate, separate the organic layer, and then carry out decompression distillation to collect 80C/ 4mmHg fraction, obtaining diethyl malonate 66~69ml (69.6g ~ 72.8g), the yield was about 87% ~ 91%.
16.0g(0.1mol) diethyl malonate and 47.0g(0.12mol) HTIB were added to an aluminum container, and heated by irradiation for 3min in a 700W microwave oven, cooled, and 19.0g of MgCl was added, and heated by irradiation for 2min, cooled, and extracted with 50ml of CH,Cl2 for two times, dried with anhydrous magnesium sulfate, and evaporated to remove the CH2Cl2 to obtain Diethyl chloromalonate. Diethyl chloromalonate 15.7g, yield 81%.
