反应详情

温度

60 °C

A mixture of 3-(3-oxo-2,3-dihydropyridazin-6-yl)-2phenylpyrazolo[1,5-a]pyridine (0.60 g), 2,2-dimethyl-3,4-epoxy-6-cyano-3,4-dihydro-2H-chromene (0.80 g), and 60% sodium hydride (0.16 g) in dimethylsulfoxide (6 ml) was stirred for 5 hours at 60° C., and then diluted with ethyl acetate. The mixture was washed with water (10 ml) and sodium chloride aqueous solution (10 ml), dried over magnesium sulfate, and evaporated in vacuo. The residue was chromatographed on silica gel (10 g) with a mixture of n-hexane and ethyl acetate (2:1). The fractions containing the object compound were combined and evaporated in vacuo. The residue was recrystallized from a mixture of ethyl acetate and diisopropyl ether to give 3-[2-(2,2-dimethyl-3-hydroxy-6-cyano-3,4-dihydro-2H-chromen-4-yl)-3-oxo-2,3-dihydropyridazin-6-yl]-2phenylpyrazolo[1,5-a]pyridine (0.51 g).

1. washThe mixture was washed with water (10 ml) and sodium chloride aqueous solution (10 ml)
2. dry with materialdried over magnesium sulfate
3. customevaporated in vacuo
4. customThe residue was chromatographed on silica gel (10 g) with a mixture of n-hexane and ethyl acetate (2:1)
5. additionThe fractions containing the object compound
6. customevaporated in vacuo
7. customThe residue was recrystallized from a mixture of ethyl acetate and diisopropyl ether