Hydrogen Bromide → 2-Fluoro-5-hydroxy-4-methylbenzoic acid
反応式
[F:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([O:12]C)=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Br>C(O)(=O)C>[F:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]参加物
4
反応条件
- 温度
- 140 °C
実験手順
To 2-fluoro-5-methoxy-4-methylbenzoic acid (650 mg, 3.53 mmol) was added 49% aqueous HBr (6.5 mL) and glacial acetic acid (5.5 mL). The mixture was heated overnight at 140° C., cooled to RT, diluted with ice water and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated to yield 2-fluoro-5-hydroxy-4-methylbenzoic acid. MS m/z=171 [M+1]+. Calc'd for C8H7FO3: 170.20.
後処理
- temperaturecooled to RT
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a6e415ee71ad401f830d8045d1f99eeb
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07880000B2
反応ノート
読み込み中…