反应详情

温度

120 °C

A total of 856 mg of (5-bromo-2-fluoro-4-methoxy-phenyl)-(3-fluoro-phenyl)-methanone obtained in Production Example II-1-b was dissolved in 13.1 ml of N,N-dimethylformamide, 185 mg of zinc cyanide, 13.6 mg of tris(dibenzylideneacetone)dipalladium and 17.4 mg of 1,1′-bis(diphenylphosphino)ferrocene were added thereto, and the mixture was stirred at 120° C. in an atmosphere of nitrogen gas for 7 hours. After cooling to room temperature, water was added to the reaction mixture and the mixture was extracted with diethyl ether. The resulting organic layer was washed with brine, dried over magnesium sulfate and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:hexane=1:2), to give 203 mg of the title compound as pale yellow crystals.

1. temperatureAfter cooling to room temperature
2. extractionthe mixture was extracted with diethyl ether
3. washThe resulting organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. customthe solvent was evaporated
6. customThe residue was purified
7. customseparated by silica gel column chromatography (ethyl acetate:hexane=1:2)