Hydrogen Bromide → 2-Bromo-4-fluoro-5-hydroxybenzaldehyde
반응식
[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([O:11]C)=[CH:6][C:3]=1[CH:4]=[O:5].Br>C(O)(=O)C>[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:7]([OH:11])=[CH:6][C:3]=1[CH:4]=[O:5]참가 물질
4
실험 절차
A solution of 2-bromo-4-fluoro-5-methoxybenzaldehyde (1.19 g, 8.20 mmol), 48% HBr (57 mL) and glacier acetic acid (57 mL) were refluxed at 130° C. for 5 hours. The glacier acetic acid was removed under reduced pressure. The solution was neutralized using sodium carbonate. Water was added and the mixture was extracted using ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and filtered. The solvent was removed under reduced pressure. The residue was purified by silica gel column using Combiflash to give 2-bromo-4-fluoro-5-hydroxybenzaldehyde (1.15 g, 64% yield).
후처리
- customThe glacier acetic acid was removed under reduced pressure
- additionWater was added
- extractionthe mixture was extracted
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customThe solvent was removed under reduced pressure
- customThe residue was purified by silica gel column
출처 및 근거
- ORD 기록
- ord-116a03750b3841c3be96ae135c32ca34
- 출처 데이터셋
- uspto-grants-2013_06
- 특허 번호
- US08461135B2
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