反应详情

温度

120 °C

A mixture of 5-chloro-2-nitrophenylamine (1.3 g, 7.0 mmol), 3-hydroxypiperidine hydrochloride (3.0 g, 20 mmol), and K2CO3 (3.0 g, 22 mmol) in DMF (10 mL) was stirred at 120° C. for 18 h. The reaction mixture was cooled to room temperature, poured into water (100 mL) and extracted with EtOAc (3×100 mL). The combined organic extracts were dried over Na2SO4, concentrated in vacuo, and purified by flash chromatography (silica gel, 4×7.5 cm, eluted with 50:50 CHCl3/EtOAc) to yield the product as an orange solid (0.89 g, 54%).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted with EtOAc (3×100 mL)
3. dry with materialThe combined organic extracts were dried over Na2SO4
4. concentrationconcentrated in vacuo
5. custompurified by flash chromatography (silica gel, 4×7.5 cm, eluted with 50:50 CHCl3/EtOAc)