反应详情

A solution of 2-chloro-3-iodopyridine (2.39 g, 10 mmol) and piperazine (8.61 g, 100 mmol) in n-BuOH, 100 mL, was stirred at reflux under N2 for 18 h. After removing most of the n-BuOH under reduced pressure, the residue was partitioned between toluene and 10% NaOH. The toluene layer was washed further with water, dried (Na2SO4), filtered and concentrated to an oil. The pyridinylpiperazine was purified by recrystallization of the dihydrochloride salt from methanol-ethanol-ethylacetate, m.p. 185°-189° C. (dec.).

1. temperatureat reflux under N2 for 18 h
2. customAfter removing most of the n-BuOH under reduced pressure
3. customthe residue was partitioned between toluene and 10% NaOH
4. washThe toluene layer was washed further with water
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated to an oil
8. customThe pyridinylpiperazine was purified by recrystallization of the dihydrochloride salt from methanol-ethanol-ethylacetate, m.p. 185°-189° C. (dec.)