反应详情

温度

115 °C

A solution of 2-fluoro-3-iodopyridine (3.052 g, 13.69 mmol), (1H-benzo[d]imidazol-2-yl)(4-hydroxyphenyl)methanone (4.89 g, 20.53 mmol) and cesium carbonate (7.58 g, 23.27 mmol) in N-Methyl-2-pyrrolidinone (20 mL) was degassed and heated to 115° C. After 64 h, the reaction was cooled to 23° C., diluted with EtOAc (250 mL) and washed with water (100 mL) and brine (75 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluant: 0.5-1.5% methanol/dichloromethane), affording the product as a yellow solid. MS (ESI, pos. ion) m/z: 404.1 (M+1).

1. temperaturethe reaction was cooled to 23° C.
2. washwashed with water (100 mL) and brine (75 mL)
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo
5. custompurified by silica gel chromatography (eluant: 0.5-1.5% methanol/dichloromethane)