反应详情

温度

95 °C

1.17 g of 4-(diphenylmethoxy)-1-piperidinepropanamine and 0.891 g of N-(6-chloro-3-methylimidazo[1,2-b]pyridazine-2-carbonyl)glycine ethyl ester were dissolved in 10 ml of 1-methyl-2-pyrrolidone; 0.517 ml of N-ethyldiisopropylamine was added, followed by stirring in an oil bath (90-100° C.) for 15 hours. After cooling, ice water was added, followed by extraction with ethyl acetate; the extract was washed with 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 (90:10:1). The desired fraction was collected and recrystallized with ethyl acetate-ethyl ether (1:1) to yield 0.629 g of the title compound.

1. temperatureAfter cooling
2. extractionfollowed by extraction with ethyl acetate
3. washthe extract was washed with saline
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. washeluted with ethyl acetate:methanol:triethylamine (90:10:1)
7. customThe desired fraction was collected
8. customrecrystallized with ethyl acetate-ethyl ether (1:1)