反应详情

温度

80 °C

To a stirred solution of 1-isopropenyl-1,3-dihydro-benzimidazol-2-one (1 g, 5.7 mmol) in DMF (50 ml) was added potassium carbonate (1.6 g, 11.5 mmol) followed by 2-fluorophenacyl bromide (1.5 g, 6.9 mmol). The resulting mixture was warmed to 80° C. for 2 h and cooled to ambient temperature. The reaction was poured into water and ethyl acetate and the layers were separated. The aqueous phase was extracted with ethyl acetate (2×) and the combined organics were dried (MgSO4). Filtration and concentration gave the crude product which was purified via column chromatography (silica gel, 50% EtOAc/hexanes). The product-containing fractions were combined and concentrated to give 1.6 g (90%) of the desired product.

1. temperaturecooled to ambient temperature
2. customthe layers were separated
3. extractionThe aqueous phase was extracted with ethyl acetate (2×)
4. dry with materialthe combined organics were dried (MgSO4)
5. filtrationFiltration and concentration
6. customgave the crude product which
7. customwas purified via column chromatography (silica gel, 50% EtOAc/hexanes)
8. concentrationconcentrated