反应详情

365 mg of 6-chloro-2-phenyl[1,2,4]triazolo[1,5-b]pyridazine and 0.513 g of 4-(diphenylmethoxy)-1-piperidinepropanamine were suspended in 8 ml of 1-butanol; 0.54 ml of N-ethyldiisopropylamine was added, followed by heating and refluxing for 19 hours. Ice water and sodium hydrogen carbonate were added, followed by extraction with ethyl acetate; the extract was washed with saturated saline, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate:methanol:triethylamine (50:5:1). The desired fraction was collected and concentrated; the resulting crystal was recrystallized from ethyl acetate to yield 308 mg of the title compound.

1. temperatureby heating
2. temperaturerefluxing for 19 hours
3. extractionfollowed by extraction with ethyl acetate
4. washthe extract was washed with saturated saline
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. washeluted with ethyl acetate:methanol:triethylamine (50:5:1)
8. customThe desired fraction was collected
9. concentrationconcentrated
10. customthe resulting crystal was recrystallized from ethyl acetate