反应详情

温度

80 °C

0.92 g of methyl 6-chloro[1,2,4]triazolo[1,5-b]pyridazine-2-carboxylate and 1.40 g of 4-(diphenylmethoxy)-1-piperidinepropanamine were suspended in 20 ml of N,N-dimethylformamide; 1.49 ml of N-ethyldiisopropylamine was added, followed by heating and refluxing at 80° C. for 15 hours. After cooling, ice water and sodium chloride were added, followed by extraction with ethyl acetate-tetrahydrofuran (1:2); 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 residue was recrystallized from ethanol-ethyl acetate (1:2) to yield 639 mg of the title compound.

1. temperatureby heating
2. temperatureAfter cooling
3. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:2)
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 residue was recrystallized from ethanol-ethyl acetate (1:2)