Iodine → HCID 178477913, 화합물
반응식
[Cl:1][C:2]1[N:7]=[C:6]2[CH:8]=[N:9][NH:10][C:5]2=[CH:4][CH:3]=1.[OH-].[K+].[I:13]I>CN(C=O)C.CCOC(C)=O.O>[Cl:1][C:2]1[N:7]=[C:6]2[C:8]([I:13])=[N:9][NH:10][C:5]2=[CH:4][CH:3]=1참가 물질
7
반응 조건
- 온도
- 0 °C
실험 절차
To a solution of 5-chloro-1H-pyrazolo[4,3-b]pyridine (100 mg, 0.65 mmol) in DMF (5 mL), was added KOH (91 mg, 1.63 mmol), I2 (247 mg, 0.98 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 5 min and then stirred at room temperature overnight. The reaction mixture was diluted with EtOAc and water. The organic phase was washed by sat. NaHSO3, dried over MgSO4, filtered, concentrated, and purified by silica gel column, eluting by 0-70% EtOAc in hexanes to give the product. LCMS-ESI+: calc'd for C6H3ClIN3: 279.9 (M+H+); Found: 279.3 (M+H+).
후처리
- stirringstirred at room temperature overnight
- washThe organic phase was washed by sat. NaHSO3
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- custompurified by silica gel column
- washeluting by 0-70% EtOAc in hexanes
- customto give the product
출처 및 근거
- ORD 기록
- ord-b3919bc976f44551b307bbbd4ecfe39c
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08987250B2
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