反应详情

温度

0 °C

To a stirred suspension of 7 (200 mg, 0.667 mmol) in THF (4 mL) at −40° C. was added 4-bromobenzyl magnesium bromide (0.25 M in Et2O, 13.3 mL, 3.34 mmol). The reaction was warmed slowly to 0° C. over 2 h. After stirring an additional 2 h, the reaction was quenched with H2O (20 mL) and extracted with EtOAc (2×20 mL). The combined organic layers were washed with brine, dried (MgSO4) and concentrated. Chromatography (SiO2, 40 to 50% EtOAc-hexane) afforded the desired product as a viscous orange oil (134 mg, 43%). ESI-MS m/z 470.2 (M++H, C19H12BrClF3N3O).

1. customthe reaction was quenched with H2O (20 mL)
2. extractionextracted with EtOAc (2×20 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated