反应详情

To a mixture of 4-(2-fluoro-4-nitrophenoxy)quinolin-7-ol (5 g, 16.7 mmol) and NaOH (6.7 g, 166.7 mmol) in acetone (67 mL) was added chloroform (21.9 g, 183.3 mmol) dropwise at room temperature. After the mixture turned brown color, the reaction was heated to reflux for 1 hour. Water (10 mL) was then added to the reaction mixture, and the resulted solution was adjusted to pH 3˜4 with 1 N HCl solution. The resulted mixture was concentrated in vacuo, and then extracted with EtOAc (30 mL). The organic phase was separated, concentrated in vacuo, and treated with 95% EtOH (10 mL). The resulted solid was collected by filtration, dried in vacuo overnight to afford the title compound as a brown solid (2.34 g, 36.4%).

1. temperaturethe reaction was heated
2. temperatureto reflux for 1 hour
3. concentrationThe resulted mixture was concentrated in vacuo
4. extractionextracted with EtOAc (30 mL)
5. customThe organic phase was separated
6. concentrationconcentrated in vacuo
7. additiontreated with 95% EtOH (10 mL)
8. filtrationThe resulted solid was collected by filtration
9. customdried in vacuo overnight