反应详情

To a solution of 3-(4-chlorophenyl)-2-isopropyl-7H-pyrano[2,3-e]indazol-4-one (20 mg, 0.059 mmol) in dry N,N-dimethylformamide (2 ml) at room temperature are added potassium hydroxide (6.3 mg, 0.112 mmol) and iodine (55 mg, in three portions over 3 h, 0.217 mmol). The reaction mixture is stirred at room temperature for 20 h, then diluted with ethyl acetate and washed successively with 10% aqueous sodium thiosulfate solution (40 ml) and saturated brine (40 ml). The organic phase is dried (MgSO4), filtered and evaporated under reduced pressure. The resulting solid is triturated with n-hexane/dichloromethane to give a colourless solid that is recovered by filtration and dried.

1. washwashed successively with 10% aqueous sodium thiosulfate solution (40 ml) and saturated brine (40 ml)
2. dry with materialThe organic phase is dried (MgSO4)
3. filtrationfiltered
4. customevaporated under reduced pressure
5. customThe resulting solid is triturated with n-hexane/dichloromethane
6. customto give a colourless solid that
7. filtrationis recovered by filtration
8. customdried