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