Methyl iodide → 5-Bromo-3-fluoro-2-methoxybenzaldehyde
反応式
[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].[C:12]([O-])([O-])=O.[Cs+].[Cs+].IC>CN(C=O)C.CCOC(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([O:10][CH3:12])=[C:6]([CH:9]=1)[CH:7]=[O:8]参加物
6
反応条件
- 温度
- 70 °C
実験手順
To a solution of 5-Bromo-3-fluoro-2-hydroxy-benzaldehyde (2.0 g, 9.13 mmol), in DMF (10 mL) was added Cs2CO3 (3.56 g, 10.95 mmol) and iodomethane (2.59 g, 18.26 mmol) and heated at 70° C. for 6 h. Reaction mixture was diluted with EtOAc (25 mL) and filtered, filtrate was washed with water, brine and dried over Na2SO4. Solvent was removed under reduced pressure and silicagel column chromatography (EtOAc:Hex, 1:3) gave pure 5-Bromo-3-fluoro-2-methoxy-benzaldehyde (2.0 g).
後処理
- customReaction mixture
- filtrationfiltered
- washfiltrate was washed with water, brine
- dry with materialdried over Na2SO4
- customSolvent was removed under reduced pressure and silicagel column chromatography (EtOAc:Hex, 1:3)
出典と根拠
- ORDレコード
- ord-93ba25c59e9046bcb3a05c670a5bcbfe
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07459472B2
反応ノート
読み込み中…