反应详情

5.57 g of 4-(diphenylmethoxy)-1-piperidinepropanamine and 3.62 g of 2-[6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3-yl]-2-methylpropionitrile were dissolved in 60 ml of 1-butanol; 5.65 ml of N-ethyldiisopropylamine was added, followed by refluxing under heating for 3.5 hours. After cooling, ethyl acetate was added; the reaction mixture was washed with saturated aqueous sodium bicarbonate, washed with saturated saline, and dried over magnesium sulfate. After concentration 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 concentrated under reduced pressure; 7.18 g of the residue was dissolved in ethanol; a solution of 1.59 g of fumaric acid in ethanol was added, followed by concentration under reduced pressure. The residue was powdered from diethyl ether and dried to yield 7.71 g of the title compound.

1. temperatureby refluxing
2. temperatureunder heating for 3.5 hours
3. temperatureAfter cooling
4. washthe reaction mixture was washed with saturated aqueous sodium bicarbonate
5. washwashed with saturated saline
6. dry with materialdried over magnesium sulfate
7. concentrationAfter concentration under reduced pressure
8. washeluted with ethyl acetate-methanol-triethylamine (50:5:1)
9. customThe desired fraction was collected
10. concentrationconcentrated under reduced pressure
11. dissolution7.18 g of the residue was dissolved in ethanol
12. additiona solution of 1.59 g of fumaric acid in ethanol was added
13. concentrationfollowed by concentration under reduced pressure
14. customdried