反应详情

温度

150 °C

After dissolving the 1,2-dibromo-4,5-diethoxy-3-fluorobenzene (480 g) in dimethylformamide (1400 ml), copper cyanide (345 g) was added and the mixture was stirred at 150° C. for 3 hours. Saturated aqueous ammonia was added to the reaction mixture, and then the mixture was stirred overnight and extraction was performed with toluene. The organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (513 g) as white crystals.

1. additionwas added
2. stirringthe mixture was stirred overnight
3. extractionextraction
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)