Iodine → HCID 178477913、化合物
反応式
[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]=1参加物
7
反応条件
- 温度
- 0 °C
実験手順
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+).
後処理
- 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
出典と根拠
- ORDレコード
- ord-b3919bc976f44551b307bbbd4ecfe39c
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987250B2
反応ノート
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