反应详情

温度

120 °C

Under a nitrogen atmosphere, to a mixture of methyl 4-((1-(4-bromo-2-methylphenyl)-4,4,4-trifluorobutyl)amino)benzoate (racemate) (1.5 g), 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex (0.285 g), N,N-diisopropylethylamine (3.65 mL), lithium acetate 2 hydrate (2.85 g) and DMF (17 mL) was added acetic anhydride (1.977 mL), and the mixture was stirred at 120° C. overnight. To the reaction mixture was added water at room temperature, and the insoluble material was filtered off through celite. The filtrate was extracted with ethyl acetate, and the extract was washed with 1M hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (725.6 mg).

1. filtrationthe insoluble material was filtered off through celite
2. extractionThe filtrate was extracted with ethyl acetate
3. washthe extract was washed with 1M hydrochloric acid and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)