反应详情

12.0 g of 2-oxiranylmethanol and 2.50 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine were dissolved in 40 ml of N,N-dimethylformamide; under ice cooling, 713 mg of 60% oily sodium hydride was added, followed by stirring at room temperature for 30 minutes. After cold saline was added, the reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1) 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 (10:1). The desired fraction was collected and concentrated under reduced pressure; the precipitated crystal was washed with diethyl ether and dried to yield 1.02 g of the title compound.

1. additionAfter cold saline was added
2. extractionthe reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1)
3. dry with materialdried over magnesium sulfate
4. concentrationAfter concentration under reduced pressure
5. washeluted with ethyl acetate-methanol (10:1)
6. customThe desired fraction was collected
7. concentrationconcentrated under reduced pressure
8. washthe precipitated crystal was washed with diethyl ether
9. customdried