反应详情

温度

70 °C

To a solution of 6-amino-5-(2,4-difluorobenzoyl)-1-(2,6-difluoro-4-hydroxyphenyl)-pyridin-2(1H)-one (300 mg, 0.79 mmol) in acetone (6 ml) under an atmosphere of nitrogen was added 1-bromo-5-chloropentane (0.115 ml, 0.87 mmol, 1.1 eq), sodium iodide (238 mg, 1.59 mmol, 2 eq) and potassium carbonate (438 mg, 3.17 mmol, 4 eq). The mixture was heated at 70° C. for 16 hours, before being allowed to cool to room temperature and partitioned between EtOAc (50 ml) and water (50 ml). The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. Purification by column chromatography (30% EtOAc in heptane) afforded a 3:2 mixture of the title compound and 6-amino-1-{4-[(5-iodopentyl)oxy]-2,6-difluorophenyl}-5-(2,4-difluorobenzoyl)pyridin-2(1H)-one (142 mg) which was used without further purification.

1. temperatureto cool to room temperature
2. custompartitioned between EtOAc (50 ml) and water (50 ml)
3. dry with materialThe organic layer was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customPurification by column chromatography (30% EtOAc in heptane)
7. customafforded