反应详情

To a solution of 100 mg (0.17 mmol) [6-bromo-5-(1-isopropyl-piperidin-4-yloxy)-1H-indol-2-yl]-[4-(piperidine-1-sulfonyl)-piperazin-1-yl]-methanone (example 1) in 3 mL acetonitrile were added 109 mg (0.33 mmol) cesium carbonate and 46 mg (0.33 mmol) isopropyl methanesulfonate. The reaction was stirred under reflux for 18 h. After cooling to room temperature, the reaction mixture was poured into 10% aqueous sodium bicarbonate solution; the phases were separated and the aqueous phase was extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue was purified by flash chromatography on silica gel with a gradient of dichloromethane:methanol (100:0 to 50:50) as eluant, to afford 60 mg (56%) of the product as a light-yellow oil.

1. temperatureunder reflux for 18 h
2. customthe phases were separated
3. extractionthe aqueous phase was extracted three times with ethyl acetate
4. washThe combined organic layers were washed with brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by flash chromatography on silica gel with a gradient of dichloromethane:methanol (100:0 to 50:50) as eluant