反应详情

0.464 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine and 1.26 g of 4-(diphenylmethoxy)-1-piperidinepropanamine were suspended in 20 ml of 1-butanol; 0.62 ml of N-ethyldiisopropylamine was added, followed by refluxing under heating for 12 hours. After ice water and sodium hydrogen carbonate were 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 washed with ethyl acetate and dried to yield 0.648 g of the title compound.

1. temperatureby refluxing
2. temperatureunder heating for 12 hours
3. extractionthe reaction mixture was extracted with ethyl acetate
4. washthe extract was washed with saturated saline
5. dry with materialdried over magnesium sulfate
6. concentrationAfter concentration under reduced pressure
7. washeluted with ethyl acetate-methanol-triethylamine (90:10:1)
8. customThe desired fraction was collected
9. concentrationconcentrated
10. customthe crystal obtained
11. washwas washed with ethyl acetate
12. customdried