反应详情

260 mg of 60% sodium hydride dispersion in mineral oil was suspended in 20 ml of tetrahydrofuran; 1.15 g of 4-(diphenylmethyl)-1-[2-(2-hydroxyethoxy)ethyl]piperazine was added, followed by heating and refluxing for 1 hour. After cooling, 540 mg of 6-chloro-7-methyl[1,2,4]triazolo[1,5-b]pyridazine was added, followed by heating and refluxing for 3 hours. After cooling, ice water was added, followed by extraction with ethyl acetate; the extract was washed with saturated saline and dried with magnesium sulfate. After the dry product was concentrated under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with dichloromethane-ethyl acetate-methanol (10:10:1). The desired fraction was collected; the crystal precipitated was collected by filtration, washed with ethyl ether and dried to yield 730 mg of the title compound.

1. temperatureby heating
2. temperaturerefluxing for 1 hour
3. temperatureAfter cooling
4. temperatureby heating
5. temperaturerefluxing for 3 hours
6. temperatureAfter cooling
7. extractionfollowed by extraction with ethyl acetate
8. washthe extract was washed with saturated saline
9. dry with materialdried with magnesium sulfate
10. concentrationAfter the dry product was concentrated under reduced pressure
11. washeluted with dichloromethane-ethyl acetate-methanol (10:10:1)
12. customThe desired fraction was collected
13. customthe crystal precipitated
14. filtrationwas collected by filtration
15. washwashed with ethyl ether
16. customdried