Iodine → 5,6-difluoro-3-iodo-1H-indole
反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[NH:7][CH:6]=[CH:5]2.[OH-].[K+].[I:14]I>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[NH:7][CH:6]=[C:5]2[I:14]参加物
5
実験手順
To a mixture of 5,6-difluoro-1H-indole (500 mg; 3.27 mmol) and KOH (458 mg; 8.18 mmol) in DMF (6.2 mL) was added a solution of iodine (837.5 mg; 3.3 mmol) in DMF (6.3 mL). The mixture was stirred at r.t. for 12 hours. It was poured into an ice-water mixture (60 mL) and extracted with EtOAc (20 mL×3). The combined organic layers was washed with brine (100 mL) and dried over anhydrous Na2SO4, filtered, concentrated to afford 930 mg (100%) of the title compound as a red solid. It was used to next step without further purification.
後処理
- extractionextracted with EtOAc (20 mL×3)
- washThe combined organic layers was washed with brine (100 mL)
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-3d92e538886041eb8e954d26d8d240fa
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09126984B2
反応ノート
読み込み中…