反应详情

4-(Diphenylmethoxy)-1-piperidinebutanamine (1.83 g) and 6-chloro[1,2,4]triazolo[1,5-b]pyridazine (557 mg) were dissolved in 1-butanol (30 ml), followed by addition of N-ethyldiisopropylamine (931 mg). The mixture was refluxed under heating for 14 hours. After being cooled, the mixture was concentrated under reduced pressure, followed by addition of ice-water and extraction with ethyl acetate. The extract was washed with an aqueous sodium chloride saturated solution, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography and eluted with a mixture of ethyl acetate, methanol and triethylamine (45:5:1). Fractions containing the objective compound were collected and concentrated. The resulting crystals were collected, washed with ethyl ether and dried to yield the title compound (149 mg).

1. temperatureThe mixture was refluxed
2. temperatureunder heating for 14 hours
3. temperatureAfter being cooled
4. concentrationthe mixture was concentrated under reduced pressure
5. additionfollowed by addition of ice-water and extraction with ethyl acetate
6. washThe extract was washed with an aqueous sodium chloride saturated solution
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. washeluted with a mixture of ethyl acetate, methanol and triethylamine (45:5:1)
10. additionFractions containing the objective compound
11. customwere collected
12. concentrationconcentrated
13. customThe resulting crystals were collected
14. washwashed with ethyl ether
15. customdried