反应详情

温度

60 °C

To a solution of 4-(benzyloxy)-1-bromo-2-methoxybenzene (2.0 g, 6.82 mmol) in THF (20 ml) was added 2-tert-butoxy-2-oxoethylzinc chloride (27.3 ml, 13.64 mmol). Nitrogen gas bubbled through the mixture for 10 min. then Pd2(dba)3 (0.312 g, 0.341 mmol) and X-PHOS (0.325 g, 0.682 mmol) were added and the resulting mixture heated at 60° C. for 30 min. The mixture was cooled, diluted with ethyl acetate (20 mL), washed with aqueous ammonium chloride (saturated, 1×15 mL), dried over MgSO4, filtered and the solvent evaporated under reduced pressure. The residue was purified by column chromatography on silica gel Biotage 50M, using a gradient eluant of EtOAc/Hexane (0-50%) to afford the title compound (2.2 g, 98%). LC/MS (m/z): 351 (M+Na)+.

1. customNitrogen gas bubbled through the mixture for 10 min.
2. temperatureThe mixture was cooled
3. washwashed with aqueous ammonium chloride (saturated, 1×15 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customthe solvent evaporated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel Biotage 50M