反应详情

温度

105 °C

A mixture of 3-bromo-2-ethyl-6-nitropyridine (2.31 g, 10.0 mmol), 2-chloropyridin-4-ol (2.59 g, 20.0 mmol) and K2CO3 (4.15 g, 30.0 mmol) in DMA (20 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 (1×), 5% LiCl (1×) and brine (1×), 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 (892 mg, 25%). MS (ESI) m/z: 280.1 (M+H+).

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