反应详情

温度

80 °C

A mixture of iodine monochioride and 2H-benzimidazole-2-one (0.67 g) (Method 59) in glacial acetic acid (8 ml) was heated to 80° C. for 1 hour then cooled. The mixture was partitioned between saturated aqueous sodium sulphite solution and DCM. The organic layer was evaporated to dryness then redissolved in ethyl acetate. The aqueous layer was extracted with ethyl acetate then all ethyl acetate extracts were combined and washed with saturated aqueous sodium hydrogen carbonate solution, water and brine. The organic extracts were passed through a Varian Chem Elut column and washed through with ethyl acetate. Volatile material was removed by evaporation to give the title compound (0.36 g) as a solid which was used without further purification. MS (ESP+): 261 (M+H)+.

1. temperaturethen cooled
2. customThe mixture was partitioned between saturated aqueous sodium sulphite solution and DCM
3. customThe organic layer was evaporated to dryness
4. dissolutionthen redissolved in ethyl acetate
5. extractionThe aqueous layer was extracted with ethyl acetate
6. washwashed with saturated aqueous sodium hydrogen carbonate solution, water and brine
7. washwashed through with ethyl acetate
8. customVolatile material was removed by evaporation