Methyl iodide → 5-Bromo-3-fluoro-2-methoxybenzaldehyde
반응식
[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]참가 물질
6
반응 조건
- 온도
- 70 °C
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-93ba25c59e9046bcb3a05c670a5bcbfe
- 출처 데이터셋
- uspto-grants-2008_12
- 특허 번호
- US07459472B2
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