反应详情

6-Chloro-2-methyl[1,2,4]triazolo[1,5-b]pyridazine (655 mg) and 4-(diphenylmethoxy)-1-piperidinepropanamine (1.26 g) was suspended in n-butanol (20 ml), followed by addition of N-ethyldiisopropylamine (1.94 ml). The mixture was refluxed under heating for 22 hours, followed by addition of ice-water and sodium hydrogen carbonate 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 silica-gel column chromatography and eluted with a mixture of ethyl acetate, methanol and triethylamine (50:5:1). Fractions containing the objective compound were collected and concentrated. The resulting crystals were washed with hexane and dried to yield the title compound (547 mg).

1. temperatureThe mixture was refluxed
2. temperatureunder heating for 22 hours
3. washThe extract was washed with an aqueous sodium chloride saturated solution
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. washeluted with a mixture of ethyl acetate, methanol and triethylamine (50:5:1)
7. additionFractions containing the objective compound
8. customwere collected
9. concentrationconcentrated
10. washThe resulting crystals were washed with hexane
11. customdried