反应详情

温度

70 °C

Under a nitrogen atmosphere, a mixture of 4,4,4-trifluoro-1-(5-phenylpyridin-2-yl)butan-1-amine (125.1 mg) obtained in step E, ethyl 4-bromobenzoate (0.214 mL), tris(dibenzylideneacetone)dipalladium (82 mg), 5-(di-tert-butylphosphino)-1′,3′,5′-triphenyl-1′H-[1,4′]bipyrazole (90 mg), sodium tert-butoxide (129 mg), tert-butanol (2.008 mL) and water (0.223 mL) was stirred at 70° 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 water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was fractionated by HPLC(C18, mobile phase: water/acetonitrile (10 mM ammonium hydrogencarbonate-containing system)). The solvent was evaporated under reduced pressure, and the residue was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (35.3 mg).

1. filtrationthe insoluble material was filtered off through celite
2. extractionThe filtrate was extracted with ethyl acetate
3. washthe extract was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customThe solvent was evaporated under reduced pressure
7. extractionthe residue was extracted with ethyl acetate
8. washThe extract was washed with water and saturated brine
9. dry with materialdried over anhydrous magnesium sulfate
10. customthe solvent was evaporated under reduced pressure