反应详情

2.56 g of 4-(diphenylmethoxy)-1-piperidinepropanamine and 1.19 g of ethyl 2-[3,6-dichloroimidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate were stirred at 160° for 3 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 (50:5:1). The desired fraction was collected and dissolved in 5 ml of ethyl acetate; 0.80 ml of a 4 N hydrogen chloride solution in ethyl acetate was added, followed by concentration. The residue was powdered by the addition of ether and dried to yield 1.33 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 (50:5:1)
7. customThe desired fraction was collected
8. dissolutiondissolved in 5 ml of ethyl acetate
9. addition0.80 ml of a 4 N hydrogen chloride solution in ethyl acetate was added
10. concentrationfollowed by concentration
11. additionThe residue was powdered by the addition of ether
12. customdried