反应详情

温度

80 °C

A mixture of 4-(4-chloro-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (300 mg, 0.94 mmol), (prepared as described for the starting material in Example 15), 1-(2-chloroethyl)-1,2-dihydro-2-pyridone (1 75 mg, 1.11 mmol), (J. Am. Chem. Soc. 1951, 73, 3635), and potassium carbonate (260 mg, 1.9 mmol) in DMF (30 ml) was heated at 80° C. for 3 hours, allowed to cool to ambient temperature and stirred for a further 18 hours. The mixture was diluted with water and extracted with ethyl acetate. The extract was washed with water, dried (MgSO4) and the solvent removed by evaporation. The residue ,as purified by column chromatography eluting with methylene chloride/methanoUtriethylamine mixtures (100/0/0 increasing to 70/30/0.5) to give 4-(4-chloro-2-fluoroanilino)-6-methoxy-7-[2-(2-oxo-1,2-dihydro-1-pyridyl)ethoxy]quinazoline (50 mg, 12%).

1. custom(prepared
2. temperatureto cool to ambient temperature
3. extractionextracted with ethyl acetate
4. washThe extract was washed with water
5. dry with materialdried (MgSO4)
6. customthe solvent removed by evaporation
7. customThe residue ,as purified by column chromatography
8. washeluting with methylene chloride/methanoUtriethylamine mixtures (100/0/0 increasing to 70/30/0.5)