反应详情

温度

40 °C

409 mg of 2-[6-[3-[4-(diphenylmethoxy)piperidino]propoxy][1,2,4]triazolo[4,3-b]pyridazin-3-yl]-2-methylpropionitrile was dissolved in 6 ml of 2-propanol; 3.5 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring under heating at an external temperature of 40° C. for 12 hours. After cooling, the 2-propanol was distilled off; the residue was extracted with ethyl acetate-tetrahydrofuran (1:1), 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; the residue was crystallized from ethyl acetate-diethyl ether (1:1), washed with diethyl ether, and dried, to yield 293 mg of the title compound.

1. temperatureAfter cooling
2. distillationthe 2-propanol was distilled off
3. extractionthe residue was extracted with ethyl acetate-tetrahydrofuran (1:1)
4. washwashed with saturated saline
5. dry with materialdried over magnesium sulfate
6. concentrationAfter concentration under reduced pressure
7. washeluted with ethyl acetate-methanol-triethylamine (50:5:1)
8. customThe desired fraction was collected
9. concentrationconcentrated under reduced pressure
10. customthe residue was crystallized from ethyl acetate-diethyl ether (1:1)
11. washwashed with diethyl ether
12. customdried