反应详情

A mixture of 4-bromo-2-fluoro-5-nitrophenol (prepared according to WO2004/014361, 10 g, 42.3 mmol) and cesium carbonate (16.42 g, 50.4 mmol) in DMF (80 mL), was stirred at room temperature and treated with benzyl bromide (5.5 g, 46.5 mmol) and the mixture was stirred/sonicated at room temperature for 2 hours (˜30 mins sonication). The DMF was evaporated and water and ethyl acetate were added and the product was extracted into ethyl acetate. The combined extracts were washed with sodium bicarbonate solution, dried (Na2SO4) and concentrated. Trituration of the solid with diethyl ether (3×) and drying gave the title compound (D4), (12.50 g).

1. customthe mixture was stirred/sonicated at room temperature for 2 hours
2. custom(˜30 mins sonication)
3. customThe DMF was evaporated
4. additionwater and ethyl acetate were added
5. extractionthe product was extracted into ethyl acetate
6. washThe combined extracts were washed with sodium bicarbonate solution
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. dry with materialTrituration of the solid with diethyl ether (3×) and drying