反应详情

0.52 g of 4-(diphenylmethoxy)-1-piperidinepropanol was dissolved in 3 ml of N,N-dimethylformamide; 0.0704 g of 60% oily sodium hydride was added, followed by stirring at room temperature for 1 hour. 0.325 g of 6-chloro-2-methyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one was added, followed by stirring at room temperature for 2 hours. After ice water was added, the reaction mixture was extracted with ethyl acetate; the extract was washed with saturated saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with ethyl acetate-methanol-triethylamine (90:10:1). The desired fraction was collected and concentrated; the crystal obtained was filtered, washed with diethyl ether, and dried, to yield 0.502 g of the title compound.

1. stirringby stirring at room temperature for 2 hours
2. extractionthe reaction mixture was extracted with ethyl acetate
3. washthe extract was washed with saturated saline
4. dry with materialdried over magnesium sulfate
5. concentrationAfter concentration under reduced pressure
6. washeluted with ethyl acetate-methanol-triethylamine (90:10:1)
7. customThe desired fraction was collected
8. concentrationconcentrated
9. customthe crystal obtained
10. filtrationwas filtered
11. washwashed with diethyl ether
12. customdried