反应详情

4-Chloro-2-fluorobenzonitrile (0.60 g, 3.9 mmol), vanillin (0.59 g, 3.9 mmol) and cesium carbonate (1.26 g, 3.9 mmol) were heated with stirring in dry DMF (4 ml) at 50° C. for 22 h. The reaction mixture was cooled, poured into water and extracted with ethyl acetate. The ethyl acetate layer was separated, washed with water, 10% aqueous sodium carbonate (2×), water (2×), brine, and dried over MgSO4. After filtration, the solvent was removed in vacuo to yield 4-chloro-2-(4-formyl-2-methoxy-phenoxy)-benzonitrile (0.98 g, 88%) as an off-white solid.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with ethyl acetate
3. customThe ethyl acetate layer was separated
4. washwashed with water, 10% aqueous sodium carbonate (2×), water (2×), brine
5. dry with materialdried over MgSO4
6. filtrationAfter filtration
7. customthe solvent was removed in vacuo