反应详情

1.41 g of 4-(diphenylmethoxy)-1-piperidinepentanamine and 0.536 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, ethyl acetate-tetrahydrofuran (2:1) was added; the mixture was washed with aqueous sodium bicarbonate and saturated 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 (185:15:2). The desired fraction was collected, dissolved in 5 ml of ethanol; a solution of 235 mg of fumaric acid in 5 ml of methanol was added, followed by concentration. Ethyl ether was added to the residue; the resulting powder was collected by filtration, washed with ethyl ether and dried to yield 0.629 g of the title compound.

1. temperatureAfter cooling
2. washthe mixture was washed with aqueous sodium bicarbonate and saturated saline
3. dry with materialdried with sodium sulfate
4. concentrationThe dry product was concentrated under reduced pressure
5. washeluted with ethyl acetate:methanol:triethylamine (185:15:2)
6. customThe desired fraction was collected
7. dissolutiondissolved in 5 ml of ethanol
8. additiona solution of 235 mg of fumaric acid in 5 ml of methanol was added
9. concentrationfollowed by concentration
10. additionEthyl ether was added to the residue
11. filtrationthe resulting powder was collected by filtration
12. washwashed with ethyl ether
13. customdried