反应详情

0.675 g of 3-[4-(diphenylmethoxy)piperidino]-2-hydroxypropylamine and 0.335 g of 6-chloro[1,2,4]triazolo [1,5-b]pyridazine were stirred at 135-140° C. for 3 hours. After cooling, aqueous sodium bicarbonate was added, followed by extraction with ethyl acetate-tetrahydrofuran (2:1); the extract was washed with saline and dried with sodium sulfate. The dry product was concentrated 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, recrystallized from ethyl acetate and dried to yield 0.509 g of the title compound.

1. temperatureAfter cooling
2. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (2:1)
3. washthe extract was washed with saline
4. dry with materialdried with sodium sulfate
5. concentrationThe dry product was concentrated under reduced pressure
6. washeluted with ethyl acetate:methanol:triethylamine (90:10:1)
7. customThe desired fraction was collected
8. customrecrystallized from ethyl acetate
9. customdried