反应详情

温度

0 °C

To a solution of 2-(4-bromophenyl)-1H-imidazole (1 equiv) in DMF (0.47 M) was added sodium hydride (3 equiv, 60% in mineral oil) at 0° C. under nitrogen. After the resulting reaction mixture was stirred at 0° C. for 15 min, (2-(chloromethoxy)-ethyl)trimethylsilane (1.1 equiv) was added. Then the mixture was stirred at room temperature for 3 h and quenched with saturated aqueous ammonium chloride solution. The aqueous layer was extracted with DCM. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and filtered. Concentration under vacuum gave the crude product, which was purified by silica gel column chromatography (25% ethyl acetate in petroleum ether) to afford the title compound (80% yield). MS (ESI) m/z 354.2 [M+1]+.

1. customAfter the resulting reaction mixture
2. stirringThen the mixture was stirred at room temperature for 3 h
3. customquenched with saturated aqueous ammonium chloride solution
4. extractionThe aqueous layer was extracted with DCM
5. washThe combined organic layers were washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationConcentration under vacuum
9. customgave the crude product, which
10. customwas purified by silica gel column chromatography (25% ethyl acetate in petroleum ether)