反应详情

温度

105 °C

A mixture of 3-bromo-2-ethyl-6-nitropyridine (3.168 g, 13.71 mmol), 2-chloro-4-hydroxypyridine (3.55 g, 27.4 mmol) and K2CO3 (5.69 g, 41.1 mmol) in DMA (25 mL) was sparged with Ar and heated at 105° C. overnight. The mixture was cooled to RT, treated with EtOAc, washed successively with 10% K2CO3, 5% LiCl, then brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford 3-((2-chloropyridin-4-yl)oxy)-2-ethyl-6-nitropyridine (1.102 g, 28%). MS (ESI) m/z: 280.0 (M+H+).

1. customwas sparged with Ar
2. temperatureThe mixture was cooled to RT
3. additiontreated with EtOAc
4. washwashed successively with 10% K2CO3, 5% LiCl
5. dry with materialbrine, dried over Na2SO4
6. concentrationconcentrated to dryness
7. custompurified via silica gel chromatography (EtOAc/Hex)