反应详情

1.41 g of 4-(diphenylmethoxy)-1-piperidinepropanamine and 1.23 g of N-(6-chloro[1,2,4]triazolo[1,5-b]pyridazine-2-carbonyl)glycine ethyl ester were dissolved in 17 ml of N,N-dimethylformamide; 1.50 ml of N-ethyldiisopropylamine was added, followed by stirring at room temperature for 28 hours, then at 60° C. for 19 hours. After cooling, aqueous sodium bicarbonate was added, followed by extraction with ethyl acetate-tetrahydrofuran (1:1); the extract was 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, concentrated, recrystallized by the addition of tetrahydrofuran, collected by filtration, washed with ethyl ether and dried to yield 987 mg of the title compound.

1. waitat 60° C. for 19 hours
2. temperatureAfter cooling
3. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:1)
4. dry with materialthe extract was dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. washeluted with ethyl acetate:methanol:triethylamine (50:5:1)
7. customThe desired fraction was collected
8. concentrationconcentrated
9. customrecrystallized by the addition of tetrahydrofuran
10. filtrationcollected by filtration
11. washwashed with ethyl ether
12. customdried