反应详情

A solution of 5-fluoro-N-methyl-2-nitroaniline (US2003-675927, 3.30 g, 19.4 mmol), 2-methoxypyridin-4-ol (2.70 g, 21.6 mmol) produced in Example (16b) and cesium carbonate (10.6 g, 32.4 mmol) in DMF (20 mL) was stirred at 80° C. for two hours. After leaving to cool, water (100 mL) was added to the reaction mixture, followed by extraction with ethyl acetate (100 mL). The organic layer was washed with water (100 mL) twice and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by silica gel chromatography (hexane/ethyl acetate, 2:1) to obtain the title compound (3.90 g, 66%) as a yellow solid.

1. customAfter leaving
2. temperatureto cool
3. extractionfollowed by extraction with ethyl acetate (100 mL)
4. washThe organic layer was washed with water (100 mL) twice
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationAfter concentration under reduced pressure
7. customthe residue was purified by silica gel chromatography (hexane/ethyl acetate, 2:1)