反应详情

温度

80 °C

A mixture of 5-fluoro-4-methyl-2-nitropyridine (0.8 g, 5.12 mmol), 4-hydroxy-2-chloropyridine (0.996 g, 7.69 mmol) and K2CO3 (0.708 g, 5.12 mmol) in DMF (10 mL) was heated at 80° C. for 4 h. The mixture was cooled to RT, poured onto water, extracted with EtOAc (2×) and the combined organics were washed with brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford 5-((2-chloropyridin-4-yl)oxy)-4-methyl-2-nitropyridine (850 mg, 62%) as an off-white solid. MS (ESI) m/z: 266.0 (M+H+).

1. temperatureThe mixture was cooled to RT
2. additionpoured onto water
3. extractionextracted with EtOAc (2×)
4. washthe combined organics were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated to dryness
7. custompurified via silica gel chromatography (EtOAc/Hex)