反应详情

4-Chloro-2,5-difluorobenzonitrile (0.45 g, 2.6 mmol), 3-hydroxy-2-methoxybenzaldehyde (0.39 g, 2.6 mmol) and cesium carbonate (0.84 g, 2.6 mmol) were heated with stirring in dry DMF (5 mL) at 50° C. for 18 h. The reaction mixture was cooled, poured into 0.1N sodium hydroxide solution and extracted with ethyl acetate. The ethyl acetate layer was separated, washed with 0.1N sodium hydroxide solution (1×), water (2×), brine (1×), and dried over MgSO4. After filtration, the solvent was removed in vacuo, and purified by chromatography to yield 4-chloro-5-fluoro-2-(3-formyl-2-methoxyphenoxy)benzonitrile (0.33 g, 42%) as a pale yellow solid.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with ethyl acetate
3. customThe ethyl acetate layer was separated
4. washwashed with 0.1N sodium hydroxide solution (1×), water (2×), brine (1×)
5. dry with materialdried over MgSO4
6. filtrationAfter filtration
7. customthe solvent was removed in vacuo
8. custompurified by chromatography