反应详情

温度

0 °C

To a solution of 1-(4-benzyloxy-3-methyl-phenyl)-ethanone (12.89 g; 53.1 mmol) in CH2Cl2 was added, dropwise, at 0° C., DIPEA (10.9 mL; 63.7 mmol) and trimethylsilyl trifluoromethanesulfonate (11.1 mL; 61.1 mmol). The resulting mixture was stirred at 0° C. for 1 hour, and subsequently, NBS (10.87 g; 61.1 mmol) was added in one portion. The mixture was allowed to warm to RT stirred overnight. Then the mixture was concentrated in vacuo, the residue dissolved in EtOAc, washed with water twice, and brine, dried (MgSO4), filtered, and concentrated in vacuo to afford 1-(4-benzyloxy-3-methyl-phenyl)-2-bromo-ethanone (11.90 g).

1. customat 0° C.
2. temperatureto warm to RT
3. stirringstirred overnight
4. concentrationThen the mixture was concentrated in vacuo
5. dissolutionthe residue dissolved in EtOAc
6. washwashed with water twice
7. dry with materialbrine, dried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo