反应详情

2,3-Difluoro-4-methylbenzonitrile (0.21 g, 1.4 mmol), 3-hydroxy-2-methoxybenzaldehyde (0.21 g, 1.4 mmol) and cesium carbonate (0.45 g, 1.4 mmol) were heated with stirring in dry DMF (4 mL) at 50° C. for 18 h. The reaction mixture was cooled, poured into 0.1N sodium hydroxide solution and extracted with diethyl ether. The ether layer was separated, washed with 0.1N sodium hydroxide solution (2×), water (3×), brine (1×), and dried over MgSO4. After filtration, the solvent was removed in vacuo, and purified by chromatography to yield 3-fluoro-2-(3-formyl-2-methoxyphenoxy)-4-methylbenzonitrile (0.12 g, 31%) as a colourless glass.

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