反应详情

温度

140 °C

A mixture of 2-bromo-4-ethoxypyridine (500 mg, 2.475 mmol), ethane-1,2-diamine (9.9 ml, 150 mmol) and potassium carbonate (685 mg, 4.95 mmol) was stirred under microwave heating at 140° C. for 2 hours. The reaction mixture was filtered, the remaining solids were rinsed with ethanol and the combined filtrates were concentrated under reduced pressure and purified by flash column chromatography (silica, gradient of 2%-100% 7N NH3 in MEOH in DCM) to yield 287 mg of a solid (1.584 mmol, 64%). MS(ESI) m/z=182.0 [M+1]+.

1. filtrationThe reaction mixture was filtered
2. washthe remaining solids were rinsed with ethanol
3. concentrationthe combined filtrates were concentrated under reduced pressure
4. custompurified by flash column chromatography (silica, gradient of 2%-100% 7N NH3 in MEOH in DCM)