N-Iodosuccinimide → 7-Fluoro-3-iodo-1H-pyrrolo[3,2-c]pyridine
반응식
[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]=1참가 물질
6
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f91460d82cc848d89c95fbe52c2bc669
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09163021B2
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