preparation | 4(1.5g,8.3mmol) was added to a 50mL eggplant bottle, 30mL phosphorus oxychloride was added to react with 2 drops of N,N-dimethylaniline at 107°C for 1h,TLC monitored the reaction completely, cooled, evaporated the solvent, and redissolved the obtained solid with dichloromethane, the saturated sodium bicarbonate aqueous solution is adjusted to pH 7, filtered to remove insoluble solids, and the dichloromethane layer and the water layer are separated. The water layer is extracted with dichloromethane twice, the dichloromethane layer is merged, and the anhydrous sodium sulfate is dried. 1.1g of white solid was obtained by column chromatography with 65% yield. |