N-Iodosuccinimide → 7-Fluoro-3-iodo-1H-pyrrolo[3,2-c]pyridine
反応式
[F:1][C:2]1[C:3]2[NH:10][CH:9]=[CH:8][C:4]=2[CH:5]=[N:6][CH:7]=1.C1C(=O)N([I:18])C(=O)C1>CN(C=O)C.O.CCOC(C)=O>[F:1][C:2]1[C:3]2[NH:10][CH:9]=[C:8]([I:18])[C:4]=2[CH:5]=[N:6][CH:7]=1参加物
6
実験手順
To a solution of 7-fluoro-pyrrolo[3,2-c]pyridine (Preparation 62, 5 g, 36.76 mmol) in anhydrous DMF (35 mL) was added NIS (9 g, 40.44 mmol), and the reaction stirred at room temperature for 4 hours. The reaction was diluted with water and EtOAc. The organic layer was collected, washed with saturate aqueous NaHCO3 solution, brine, dried over sodium sulphate and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 50-100% EtOAc in heptanes followed by 5% MeOH in DCM to afford the title compound (5 g).
後処理
- customThe organic layer was collected
- washwashed with saturate aqueous NaHCO3 solution, brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated in vacuo
- customThe residue was purified
- washeluting with 50-100% EtOAc in heptanes
出典と根拠
- ORDレコード
- ord-f91460d82cc848d89c95fbe52c2bc669
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09163021B2
反応ノート
読み込み中…