反应详情

温度

110 °C

Into a 100-mL round-bottom flask, was placed methyl 2-(4-fluorophenyl)-3-oxo-1,2,3,4-tetrahydroquinoxaline-6-carboxylate (1.2 g, 4.00 mmol, 1.00 equiv), POCl3 (12.2 g, 80.26 mmol, 20.00 equiv), N,N-dimethylbenzenamine (4.9 g, 40.50 mmol, 10.00 equiv). The resulting solution was stirred for overnight at 110° C. in an oil bath. The resulting mixture was concentrated under vacuum and diluted with 50 mL of water. The pH of the aqueous solution was adjusted to 7 with sodium bicarbonate (4M). The resulting mixture was concentrated under vacuum and purified by silica gel chromatography with ethyl acetate/petroleum ether (1:40). This resulted in 0.5 g (40%) of methyl 3-chloro-2-(4-fluorophenyl)quinoxaline-6-carboxylate as a white solid.

1. customInto a 100-mL round-bottom flask, was placed
2. concentrationThe resulting mixture was concentrated under vacuum
3. additiondiluted with 50 mL of water
4. concentrationThe resulting mixture was concentrated under vacuum
5. custompurified by silica gel chromatography with ethyl acetate/petroleum ether (1:40)
6. customThis resulted in 0.5 g (40%) of methyl 3-chloro-2-(4-fluorophenyl)quinoxaline-6-carboxylate as a white solid