反应详情

4-(Diphenylmethoxy)-1-piperidineethanol (740 mg) was dissolved in dried tetrahydrofurane (18 ml), followed by addition of sodium t-butoxide (251 mg). The mixture was refluxed under heating for 25 minutes. After the mixture was cooled, 7-tert-butyl-6-chloro[1,2,4]triazolo[1,5-b]pyridazine (501 mg) was added thereto. The mixture was refluxed under heating for 2 hours. After the mixture was cooled, ice-water was added thereto, followed by 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 ethyl acetate. Fractions containing the objective compound were collected and recrystallized from ethyl acetate to yield the title compound (380 mg).

1. temperatureThe mixture was refluxed
2. temperatureunder heating for 25 minutes
3. temperatureAfter the mixture was cooled
4. temperatureThe mixture was refluxed
5. temperatureunder heating for 2 hours
6. temperatureAfter the mixture was cooled
7. extractionfollowed by extraction with ethyl acetate
8. washThe extract was washed with an aqueous sodium chloride saturated solution
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated under reduced pressure
11. washeluted with ethyl acetate
12. additionFractions containing the objective compound
13. customwere collected
14. customrecrystallized from ethyl acetate