反应详情

温度

180 °C

5.33 g of 5-bromo-2-fluoro-4-methoxy-benzaldehyde was dissolved in 73 ml of 1-methyl-2-pyrrolidone, 2.46 g of copper cyanide was added under stirring at 180° C. for 5.5 hours. After cooling to room temperature, water was added to the reaction mixture. The mixture was extracted with ethyl acetate and filtered through Celite. Then, the resulting organic layer was washed with water and brine, dried over magnesium sulfate and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography, to give 0.983 g of the title compound as pale yellow crystals.

1. temperatureAfter cooling to room temperature
2. extractionThe mixture was extracted with ethyl acetate
3. filtrationfiltered through Celite
4. washThen, the resulting organic layer was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. customthe solvent was evaporated
7. customThe residue was purified
8. customseparated by silica gel column chromatography