反应详情

温度

80 °C

A mixture of 2-fluoro-3-iodopyridine (4.93 g, 22.11 mmol), 4-(benzo[d]thiazol-2-ylamino)phenol (6.16 g, 25.4 mmol), and cesium carbonate (10.81 g, 33.2 mmol) in DMSO (50 mL) was heated at 80° C. overnight. The reaction was cooled to rt and poured into water (200 mL). The solution was extracted with EtOAc (3×) and the combined organic layers were washed with brine, evaporated onto silica gel and purified by flash chromatography (Isco (240 gram)) eluting with EtOAc:hexanes (0:1→1:1) to give a white crystalline solid. MS (ESI, pos. ion) m/z: 445.8 (M+1).

1. temperatureThe reaction was cooled to rt
2. extractionThe solution was extracted with EtOAc (3×)
3. washthe combined organic layers were washed with brine
4. customevaporated onto silica gel
5. custompurified by flash chromatography (Isco (240 gram))
6. washeluting with EtOAc:hexanes (0:1→1:1)
7. customto give a white crystalline solid