反応 #42779

反応方程式

3-(4-chlorophenyl)-2-isopropyl-7H-pyrano[2,3-e]indazol-4-one

potassium hydroxide

iodine

→

3-(4-Chlorophenyl)-9-iodo-2-isopropyl-7H-pyrano[2,3-e]indazol-4-one

溶媒

N,N-dimethylformamide

ethyl acetate

反応条件

後処理

1. 1
   洗浄washed successively with 10% aqueous sodium thiosulfate solution (40 ml) and saturated brine (40 ml)
2. 2
   乾燥The organic phase is dried (MgSO4)
3. 3
   ろ過filtered
4. 4
   その他evaporated under reduced pressure
5. 5
   その他The resulting solid is triturated with n-hexane/dichloromethane
6. 6
   その他to give a colourless solid that
7. 7
   ろ過is recovered by filtration
8. 8
   その他dried

実験手順

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.

出典