N-Iodosuccinimide → 1-(5-Chloro-4-fluoro-2-hydroxy-3-iodophenyl)ethanone
反応式
[Cl:1][C:2]1[C:3]([F:12])=[CH:4][C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.[I:13]N1C(=O)CCC1=O>C(O)(=O)C>[Cl:1][C:2]1[C:3]([F:12])=[C:4]([I:13])[C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
A solution of 1-(5-chloro-4-fluoro-2-hydroxyphenyl)ethanone (23.8 g, 126 mmol) in acetic acid (100 mL) was treated with N-iodosuccinimide (34.1 g, 151 mmol) and stirred at 70° C. for 2 hours. The reaction mixture was concentrated, diluted with EtOAc and quenched with sat. NaHCO3 solution. The organic layer was separated, washed with water, dried over MgSO4 and concentrated under reduced pressure to give the desired product to be used in the next step without further purification.
後処理
- concentrationThe reaction mixture was concentrated
- additiondiluted with EtOAc
- customquenched with sat. NaHCO3 solution
- customThe organic layer was separated
- washwashed with water
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-8fcb8817adc1452aba252d85dc052234
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096600B2
反応ノート
読み込み中…