反应详情

4.2 g of 4-(diphenylmethoxy)-1-piperidinepropaneamine and 1.76 g of ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate were stirred at 192-200° C. for 3.5 hours. After cooling, an aqueous sodium bicarbonate solution was added thereto and extracted with ethyl acetate. The extract was washed with a brine solution, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to be eluted with ethyl acetate:methanol:triethyl amine (100:5:1). The desired fraction was collected and dissolved in 16 mL of ethyl acetate, and a solution prepared by dissolving 867 mg of fumaric acid in 16 mL of methanol was added thereto, followed by concentration. To the residue was added acetone and the crystals formed were collected by filtration, washed with acetone and dried to provide 2.30 g of the title compound.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate
3. washThe extract was washed with a brine solution
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. washto be eluted with ethyl acetate:methanol:triethyl amine (100:5:1)
7. customThe desired fraction was collected
8. dissolutiondissolved in 16 mL of ethyl acetate
9. customa solution prepared
10. additionwas added
11. concentrationfollowed by concentration
12. additionTo the residue was added acetone
13. customthe crystals formed
14. filtrationwere collected by filtration
15. washwashed with acetone
16. customdried