反应详情

温度

60 °C

0.311 g of 4-(diphenylmethyl)-1-piperazinepropanol was dissolved in 5 ml of N,N-dimethylformamide; 0.048 g of 60% oily sodium hydride was added; the reaction mixture was stirred in an oil bath (60° C.) for 30 minutes. After cooling, 0.232 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine was added; the reaction mixture was stirred in an oil bath. (bath temperature 60° C.) for 40 minutes. After cooling, ice water was added; the reaction mixture was extracted with ethyl acetate; the extract was washed with 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 (90:10:1). The desired fraction was collected and concentrated; the crystal obtained was filtered, washed with ethyl ether, and dried, to yield 0.339 g of the title compound.

1. temperatureAfter cooling
2. stirringthe reaction mixture was stirred in an oil bath
3. wait(bath temperature 60° C.) for 40 minutes
4. temperatureAfter cooling
5. extractionthe reaction mixture was extracted with ethyl acetate
6. washthe extract was washed with saline
7. dry with materialdried over magnesium sulfate
8. concentrationAfter concentration under reduced pressure
9. washeluted with ethyl acetate-methanol-triethylamine (90:10:1)
10. customThe desired fraction was collected
11. concentrationconcentrated
12. customthe crystal obtained
13. filtrationwas filtered
14. washwashed with ethyl ether
15. customdried