反应详情

温度

5 °C

To a solution of ethyl 3-(1-(4-bromobenzyl)-6-methoxy-1H-benzo[d]imidazol-2-yl)-2,2-dimethylpropanoate (12 g, 27 mmol) in DCM (200 mL) was added BBr3 (20 g, 81 mmol) in DCM (100 mL) drop wise at −78° Celsius. The solution was gradually warmed to 5° Celsius and stirred for 3 h. The reaction mixture was slowly added to saturated NaHCO3 with rapid stirring for 1 h. The organic phase was separated and aqueous phase was extracted with DCM (200 mL). The combined organic phases were dried over Na2SO4, filtered, concentrated to dryness and purified by FCC to provide the title compound. MS (ESI): mass calcd. for C21H23BrN2O3, 430.09; m/z found, 438 [M+H]+.

1. stirringwith rapid stirring for 1 h
2. customThe organic phase was separated
3. extractionaqueous phase was extracted with DCM (200 mL)
4. dry with materialThe combined organic phases were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. custompurified by FCC