反应详情

4-Chloro-2-fluorobenzonitrile (0.35 g, 2.2 mmol), 2-ethoxy-3-hydroxybenzaldehyde (0.37 g, 2.2 mmol) and cesium carbonate (0.73 g, 2.2 mmol) were heated with stirring in dry DMF (4 mL) at 50° C. for 19 h. The reaction mixture was cooled, poured into water and extracted with ethyl acetate. The ethyl acetate layer was separated, washed with 1N sodium hydroxide solution (2×), water (2×), brine (1×), and dried over MgSO4. After filtration, the solvent was removed in vacuo to yield 4-chloro-2-(2-ethoxy-3-formylphenoxy)benzonitrile (0.55 g, 82%) as a tan solid.

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