反应详情

温度

80 °C

To a mixture of tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3,6-dihydropyridine-1(2H)-carboxylate (3.16 g), 4-bromo-3-methoxy-1-nitrobenzene (2.63 g) and DMF (31.6 mL), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II), dichloromethane adduct (0.50 g) and potassium carbonate (4.24 g) were added and stirred at 80° C. for 4 hours. After this mixture was concentrated under reduced pressure, water and ethyl acetate were added, and insoluble materials were filtered through celite. The organic layer was washed with saturated aqueous sodium chloride. After drying over anhydrous magnesium sulfate, the solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=1:0 to 2:1) to give tert-butyl 4-(2-methoxy-4-nitrophenyl)-3,6-dihydropyridine-1(2H)-carboxylate (2.21 g) as a yellow solid.

1. additionwere added
2. concentrationAfter this mixture was concentrated under reduced pressure, water and ethyl acetate
3. additionwere added
4. filtrationinsoluble materials were filtered through celite
5. washThe organic layer was washed with saturated aqueous sodium chloride
6. dry with materialAfter drying over anhydrous magnesium sulfate
7. distillationthe solvent was distilled off
8. customthe residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=1:0 to 2:1)