反应详情

A solution of 2-chloro-3-nitropyridine (4.76 g, 30 mmol) and piperazine (5.9, 69 mmol) in acetonitrile, (75 mL), was stirred at reflux for 5 h. After concentrating under reduced pressure, the residue was partitioned between ethyl acetate and 10% NaOH. The ethyl acetate extract was washed with water, dried (Na2SO4), filtered and concentrated. Flash chromatography over Al2O3 and elution with 2% MeOH-98% CHCl3 afforded the title compound, m.p. 82°-87° C. An analytical sample, m.p. 83.5°-86.5° C., was obtained upon recrystallization from CHCl3 -hexane.

1. temperatureat reflux for 5 h
2. concentrationAfter concentrating under reduced pressure
3. customthe residue was partitioned between ethyl acetate and 10% NaOH
4. extractionThe ethyl acetate extract
5. washwas washed with water
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. washFlash chromatography over Al2O3 and elution with 2% MeOH-98% CHCl3