反应详情

4.2 g of 4-(diphenylmethoxy)-1-piperidinepropanamine and 1.76 g of ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate were stirred at 190-200° C. for 3.5 hours. After cooling, aqueous sodium bicarbonate 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:triethylamine (100:5:1). The desired fraction was collected, dissolved in 16 ml of ethyl acetate; a solution of 867 mg of fumaric acid in 16 ml of methanol was added, followed by concentration. Acetone was added to the residue; the crystal precipitated was collected by filtration, washed with acetone and dried to yield 2.30 g of the title compound.

1. temperatureAfter cooling
2. extractionfollowed by extraction with ethyl acetate
3. washthe extract was washed with saturated saline
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. washeluted with ethyl acetate:methanol:triethylamine (100:5:1)
7. customThe desired fraction was collected
8. dissolutiondissolved in 16 ml of ethyl acetate
9. additiona solution of 867 mg of fumaric acid in 16 ml of methanol was added
10. concentrationfollowed by concentration
11. additionAcetone was added to the residue
12. customthe crystal precipitated
13. filtrationwas collected by filtration
14. washwashed with acetone
15. customdried