反应详情

温度

60 °C

To a solution of 5-(benzyloxy)-2-bromobenzonitrile (0.73 g, 2.53 mmol) in THF (10 ml) was added 2-tert-butoxy-2-oxoethylzinc chloride (10.13 ml, 5.07 mmol). Nitrogen gas bubbled through the mixture for 10 min. then Pd2(dba)3 (0.116 g, 0.127 mmol) and X-PHOS (0.121 g, 0.253 mmol) were added and the resulting mixture heated at 60° C. for 50 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 (0-15%) to afford the title compound. LC/MS (m/z): 346 (M+H)+.

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