反应详情

温度

60 °C

1.5 equivalents of sodium methoxide (30% in methanol) were added to a suspension of 13.4 g of acetamidine hydrochloride in 150 ml of ethanol. The precipitate was filtered off and washed with 100 ml of ethanol. Additional 1.5 equivalents of sodium methoxide (30% in methanol) were added to the filtrate. Then a solution of 39.3 g of 2-(2-chloro-5-fluoro-benzoylamino)malonic acid diethyl ester in 100 ml of ethanol was added dropwise. The reaction mixture was stirred at 60° C. for 2 h. After cooling to 0° C. for 30 min, the precipitate was filtered off with suction, washed with 100 ml of a solution of hydrogen chloride in isopropanol and dried to give 35.7 g of the title compound.

1. filtrationThe precipitate was filtered off
2. washwashed with 100 ml of ethanol
3. temperatureAfter cooling to 0° C. for 30 min
4. filtrationthe precipitate was filtered off with suction
5. washwashed with 100 ml of a solution of hydrogen chloride in isopropanol
6. customdried