反应详情

温度

155 °C

To a solution of 1-bromo-3,4-diethoxy-2-fluorobenzene (12.0 g, 45.6 mmoL) in N,N-dimethylformamide (DMF) (60 mL), copper (I) cyanide (6.8 g, 68.3 mmoL) was added at room temperature and then stirred at 155° C. for 3 hours. After ice cooling the reaction solution, ethyl acetate and 28% aqueous ammonium were added thereto to separate the organic layer. This organic layer was washed with water and saturated saline and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated. The residue was purified by silica gel column chromatography (n-hexane, ethyl acetate) to give 9.0 g of the captioned compound (yield: 94.3%).

1. customto separate the organic layer
2. washThis organic layer was washed with water and saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationAfter filtration
5. customthe solvent was evaporated
6. customThe residue was purified by silica gel column chromatography (n-hexane, ethyl acetate)