Hydrogen Bromide → 2-Bromo-4-fluoro-5-hydroxybenzaldehyde
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-3a121b9442ea4491b7f7688a2f8bd8ec
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09012431B2
反応ノート
読み込み中…