反应详情

温度

60 °C

991 mg of 4-(diphenylmethoxy)-1-piperidinepropanol was dissolved in 20 ml of tetrahydrofuran; 322 mg of sodium tert-butoxide was added, followed by stirring at an external temperature of 60° C. for 2 hours. After cooling, 642 mg of 3-tert-butyl-6-chloro[1,2,4]triazolo[4,3-b]pyridazine was added, followed by refluxing under heating for 2 hours. After cooling, saline was added; the reaction mixture was extracted with ethyl acetate 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; 1.26 g of the residue was dissolved in 3 ml of pyridine; 1.5 ml of acetic anhydride was added, followed by stirring at room temperature for 6 hours. After the reaction mixture was concentrated 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 crystallized from ethyl acetate-diethyl ether (1:1), washed with diethyl ether, and dried, to yield 500 mg of the title compound.

1. temperatureAfter cooling
2. temperatureby refluxing
3. temperatureunder heating for 2 hours
4. temperatureAfter cooling
5. additionsaline was added
6. extractionthe reaction mixture was extracted with ethyl acetate
7. dry with materialdried over magnesium sulfate
8. concentrationAfter concentration under reduced pressure
9. washeluted with ethyl acetate-methanol-triethylamine (50:5:1)
10. customThe desired fraction was collected
11. concentrationconcentrated under reduced pressure
12. dissolution1.26 g of the residue was dissolved in 3 ml of pyridine
13. addition1.5 ml of acetic anhydride was added
14. stirringby stirring at room temperature for 6 hours
15. concentrationAfter the reaction mixture was concentrated under reduced pressure
16. washeluted with ethyl acetate-methanol-triethylamine (50:5:1)
17. customThe desired fraction was collected
18. concentrationconcentrated under reduced pressure
19. customthe residue crystallized from ethyl acetate-diethyl ether (1:1)
20. washwashed with diethyl ether
21. customdried