反应详情

150 mg of 60% sodium hydride in oil was suspended in 20 ml of tetrahydrofuran; 1.05 g of [2-[4-(diphenylmethyl)-1-piperazinyl]ethoxy]ethanol was added, followed by heating and refluxing for 1 hour. After cooling, 650 mg of 7-t-butyl-6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added, followed by heating and refluxing for 2 hours. After cooling, ice water was added, followed by extraction with ethyl acetate; the extract was washed with saturated saline, dried over magnesium sulfate and 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; the residue was dissolved in 5 ml of ethyl acetate; 2.1 ml of a 4N hydrogen chloride solution in ethyl acetate was added; the crystal precipitated was collected by filtration, washed with ethyl ether and dried to yield 1.55 g of the title compound.

1. temperatureby heating
2. temperaturerefluxing for 1 hour
3. temperatureAfter cooling
4. temperatureby heating
5. temperaturerefluxing for 2 hours
6. temperatureAfter cooling
7. extractionfollowed by extraction with ethyl acetate
8. washthe extract was washed with saturated saline
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated under reduced pressure
11. washeluted with ethyl acetate:methanol (10:1)
12. customThe desired fraction was collected
13. dissolutionthe residue was dissolved in 5 ml of ethyl acetate
14. addition2.1 ml of a 4N hydrogen chloride solution in ethyl acetate was added
15. customthe crystal precipitated
16. filtrationwas collected by filtration
17. washwashed with ethyl ether
18. customdried