反应详情

温度

120 °C

To a suspension of 6-bromo-3-(4-chlorophenoxy)-4-(trifluoromethyl)quinolin-2(1H)-one (1.08 g, 2.58 mmol, Intermediate 7, step c) in phosphoryl trichloride (7.2 mL, 77.3 mmol) was added diisopropylethylamine (1.33 mL, 7.74 mmol). The resulting mixture was heated at 120° C. for 8 hours. The solution was concentrated in vacuo at room temperature and the resulting residue was cooled to 0° C. with an ice bath. To the cold residue was added ice in small portions to quench excess phosphoryl trichloride. After cessation of bubbling, the solid suspension was diluted with dichloromethane. The organic phase was separated out, dried (MgSO4), filtered and concentrated to yield the title compound.

1. concentrationThe solution was concentrated in vacuo at room temperature
2. temperaturethe resulting residue was cooled to 0° C. with an ice bath
3. additionTo the cold residue was added ice in small portions
4. customto quench excess phosphoryl trichloride
5. customAfter cessation of bubbling
6. additionthe solid suspension was diluted with dichloromethane
7. customThe organic phase was separated out
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated