反应详情

温度

190 °C

A mixture containing 4-chloro-2-aminopyridine (164; 26 g, 0.20 mol), K2CO3 (0.40 mol) and morpholine (48; 0.6 mol) in DMSO (150 mL) was stirred at 190° C. for 10 h. Upon cooling to room temperature, the reaction mixture was diluted with water (300 mL) and the resulting mixture was extracted with ethyl acetate (4×150 mL). The combined organic layers were washed with water (3×25 mL), dried (Na2SO4) and concentrated under reduced pressure. The resulting residue was purified by chromatography (petroleum ether:ethyl acetate=10:1) to afford 6-morpholinopyridin-2-amine 165 (17 g, 47%) as a white solid.

1. temperatureUpon cooling to room temperature
2. extractionthe resulting mixture was extracted with ethyl acetate (4×150 mL)
3. washThe combined organic layers were washed with water (3×25 mL)
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by chromatography (petroleum ether:ethyl acetate=10:1)