Hydrogen Bromide → 4-Bromo-3-fluoro-2-hydroxybenzaldehyde
反応式
Br.[Br:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[O:8])=[C:5]([O:11]C)[C:4]=1[F:13]>C(O)(=O)C>[Br:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[O:8])=[C:5]([OH:11])[C:4]=1[F:13]参加物
4
反応条件
- 温度
- 120 °C
実験手順
48% Hydrobromic acid (254 mL) was added to a solution of 4-bromo-3-fluoro-2-methoxybenzaldehyde (52.3 g) in acetic acid (350 mL) at room temperature. The mixture was stirred at 120° C. under nitrogen atmosphere for 16 hours and concentrated in vacuo. The residue was diluted with ethyl acetate and water. The mixture was extracted with ethyl acetate. The organic layer was separated, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was triturated with diisopropyl ether and collected by filtration to give the title compound (34.6 g).
後処理
- concentrationconcentrated in vacuo
- additionThe residue was diluted with ethyl acetate and water
- extractionThe mixture was extracted with ethyl acetate
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
- customThe residue was triturated with diisopropyl ether
- filtrationcollected by filtration
出典と根拠
- ORDレコード
- ord-e9cf6a8b69c14685bccbcb8f137f21d5
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09353108B2
反応ノート
読み込み中…