反应详情

温度

80 °C

A mixture of 7-[(4-chlorophenyl)(isopropyl)amino]-1-methyl-1,3-dihydro-2H-benzimidazol-2-one (42 mg, 0.13 mmol) and phosphorous oxychloride (1.5 ml) was stirred at 80° C. for 1.5 h. The mixture was concentrated in vacuo and quenched with saturated aqueous sodium bicarbonate (10 ml) and extracted with ethyl acetate (20 ml). The extract was washed with water, dried over magnesium sulfate and evaporated. The residue was flash chromatographed eluting with a 17% ethyl acetate/hexanes to give 31.9 mg (72%) of the title compound as an oil.

1. concentrationThe mixture was concentrated in vacuo
2. customquenched with saturated aqueous sodium bicarbonate (10 ml)
3. extractionextracted with ethyl acetate (20 ml)
4. washThe extract was washed with water
5. dry with materialdried over magnesium sulfate
6. customevaporated
7. customchromatographed
8. washeluting with a 17% ethyl acetate/hexanes