反应详情

温度

120 °C

A suspension of 2-fluoro-3-iodopyridine (1.674 g, 7.51 mmol), 4-(benzo[d]thiazol-2-ylamino)phenol (2.73 g, 11.26 mmol) and cesium carbonate (4.16 g, 12.76 mmol) in N-methyl-2-pyrrolidinone (10 mL) was degassed and heated to 120° C. After 3 h 30 min, the reaction was cooled to 23° C., diluted with EtOAc (200 mL) and washed with water (100 mL) and brine (100 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluant: 0-1% methanol/dichloromethane), affording the product as an off-white solid. MS (ESI, pos. ion) m/z: 445.9 (M+1).

1. customwas degassed
2. temperaturethe reaction was cooled to 23° C.
3. additiondiluted with EtOAc (200 mL)
4. washwashed with water (100 mL) and brine (100 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. custompurified by silica gel chromatography (eluant: 0-1% methanol/dichloromethane)