Iodine → 3-Iodo-5-nitro-1H-indole
反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][CH:8]=[CH:7]2)([O-:3])=[O:2].[OH-].[K+].[I:15]I.S(=O)(=O)(O)[O-].[Na+]>CN(C=O)C>[I:15][C:7]1[C:6]2[C:10](=[CH:11][CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[NH:9][CH:8]=1参加物
6
実験手順
To a solution of 5-nitro-1H-indole (5 g, 30.86 mmol) in DMF (50 mL) was added KOH (5 g, 92.58 mmol), followed by addition of I2 (15.7 g, 61.74 mmol). The reaction mixture was stirred at RT for 2 h and then added 10% aqueous sodium bisulfate (50 mL) solution. The resulting precipitate was collected by filtration, washed with water and dried under vacuum to obtain the title compound as a pale yellow solid (8.0 g. 91%). MS (ESI, pos. ion) m/z: 286.9 (M−1)
後処理
- filtrationThe resulting precipitate was collected by filtration
- washwashed with water
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-ff0d112a858840b8b45af04f98f8b228
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09090593B2
反応ノート
読み込み中…