反应详情

The solid 6-bromo-quinolin-4-ol (52 g, 232.1 mmol) was added to phosphorus oxychloride (213.5 mL) and then the mixture was heated to reflux for 6 h to afford a light brown solution. After cooling to room temperature, the excess phosphorus oxychloride was removed under the vacuum. The remaining residue was poured into an ice-containing beaker (2 L). Then, it was slowly neutralized with solid potassium carbonate and the resulting solids were collected by filtration and washed with water. After drying in air, 55.46 g (98.5% yield) of 6-bromo-4-chloro-quinoline was isolated as a light yellow solid: EI-HRMS m/e calcd for C9H5BrClN (M+) 240.9294, found 240.9297.

1. temperaturethe mixture was heated
2. temperatureto reflux for 6 h
3. customto afford a light brown solution
4. customthe excess phosphorus oxychloride was removed under the vacuum
5. additionThe remaining residue was poured into an ice-
6. additioncontaining beaker (2 L)
7. filtrationthe resulting solids were collected by filtration
8. washwashed with water
9. customAfter drying in air