反应详情

温度

155 °C

Copper(I)cyanide (6.8 g, 68.3 mmol) was added to a solution of 1-bromo-3,4-diethoxy-2-fluorobenzene (12.0 g, 45.6 mmol) in N,N-dimethylformamide (DMF) (60 mL) at room temperature, and this was then stirred at 155° C. for 3 hours. The reaction solution was cooled on ice. Following addition of ethyl acetate and 28% aqueous ammonia, the organic layer was separated and washed with water and saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was removed after filtration, and the residue was purified by silica gel column chromatography (n-hexane, ethyl acetate) to give 9.0 g of the subject compound (yield: 94.3%).

1. temperatureThe reaction solution was cooled on ice
2. customthe organic layer was separated
3. washwashed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was removed
6. filtrationafter filtration
7. customthe residue was purified by silica gel column chromatography (n-hexane, ethyl acetate)