反应详情

A mixture of 6-(2-methoxyphenyl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (0.28 g), lithium iodide (0.44 g) and collidine (0.79 g) was refluxed for 5 hours. Under reduced pressure, collidine was evaporated, and the residue was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give, the residue was purified with silica gel column chromatography (EtOAc/hexane). The resulting crystals were recrystallized from acetone-hexane to give colorless crystals of 6-(2-hydroxyphenyl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (0.05 g).

1. temperaturewas refluxed for 5 hours
2. customUnder reduced pressure, collidine was evaporated
3. extractionthe residue was extracted with ethyl acetate
4. washThe organic layer was washed with water and saturated brine
5. dry with materialdried with magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customto give
8. customthe residue was purified with silica gel column chromatography (EtOAc/hexane)
9. customThe resulting crystals were recrystallized from acetone-hexane