反应详情

温度

95 °C

1.90 g of 4-(diphenylmethoxy)-1-piperidinepropanamine and 1.38 g of N-(6-chloroimidazo-[1,2-b]pyridazine-2-carbonyl)glycine ethyl ester were dissolved in 15 ml of 1-methyl-2-pyrrolidone; 0.841 ml of N-ethyldiisopropylamine was added, followed by stirring in an oil bath (90-100° C.) for 24 hours. After cooling, ice water and saline were added, followed by extraction with ethyl acetate; the extract was washed with saturated saline and dried with magnesium 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 (95:5:1). The desired fraction was collected and recrystallized from ethyl acetate to yield 1.28 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 with magnesium sulfate
5. concentrationThe dry product was concentrated under reduced pressure
6. washeluted with ethyl acetate:methanol:triethylamine (95:5:1)
7. customThe desired fraction was collected
8. customrecrystallized from ethyl acetate