反应详情

653 mg of 4-(diphenylmethoxy)-1-piperidinepropanol was dissolved in 10 ml of N,N-dimethylformamide; 88 mg of a 60% dispersion of sodium hydride in mineral oil was added, followed by stirring at room temperature under reduced pressure for 1.5 hours. To the reaction mixture, 483 mg of isopropyl (6-chloro[1,2,4]triazolo[1,5-b]pyridazin-2-yl)carboxylate was added under ice cooling conditions, followed by stirring at constant temperature for 3.5 hours. Ice water was added, followed by extraction with ethyl acetate-tetrahydrofuran (1:1); the extract was washed with saturated saline and dried with magnesium sulfate. The dry product was concentrated under reduced pressure; the residue was subjected to silica gel column chromatography and eluted with ethyl acetate:methanol (10:1). The desired fraction was collected and concentrated; the crystal precipitated was washed with ethyl ether, collected by filtration and dried to yield 462 mg of the title compound.

1. stirringby stirring at constant temperature for 3.5 hours
2. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:1)
3. washthe extract was washed with saturated saline
4. dry with materialdried with magnesium sulfate
5. concentrationThe dry product was concentrated under reduced pressure
6. washeluted with ethyl acetate:methanol (10:1)
7. customThe desired fraction was collected
8. concentrationconcentrated
9. customthe crystal precipitated
10. washwas washed with ethyl ether
11. filtrationcollected by filtration
12. customdried