反应详情

温度

130 °C

Solid anhydrous magnesium bromide (3.66 g, 19.9 mmol) was carefully added to a stirred solution of 4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazoline-6-carbaldehyde (2.0 g, 6.04 mmol) in pyridine (30 ml) at room temperature. The resulting suspension was heated at 130° C. for 16 hours, cooled to room temperature and concentrated to dryness to give a yellow solid. This was suspended in water (100 ml), collected by filtration and washed several times with water. The resulting yellow solid was dried to a constant weight in a vacuum oven at 40° C. to give 4-[(3-chloro-2-fluorophenyl)amino]-7-hydroxyquinazoline-6-carbaldehyde, (1.93 g, 100%); Mass Spectrum: (M+H)+ 318.

1. temperaturecooled to room temperature
2. concentrationconcentrated to dryness
3. customto give a yellow solid
4. filtrationcollected by filtration
5. washwashed several times with water
6. customThe resulting yellow solid was dried to a constant weight in a vacuum oven at 40° C.