N-bromobutanimide → 3-bromo-5-fluoro-2-methylbenzoic acid
反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[Br:12]N1C(=O)CCC1=O>S(=O)(=O)(O)O>[Br:12][C:4]1[C:5]([CH3:11])=[C:6]([CH:10]=[C:2]([F:1])[CH:3]=1)[C:7]([OH:9])=[O:8]参加物
4
反応条件
- 温度
- 0 °C
実験手順
To a cooled (0° C.) solution of 5-fluoro-2-methyl-benzoic acid (20 g, 130 mmol) in conc. sulfuric acid (200 mL) was added N-bromosuccinimide (24.3 g, 136 mmol) portionwise. The resulting mixture was stirred at 0° C. for 3 hrs, then warmed to room temperature and stirred for 16 hrs. Then the mixture was poured slowly into ice water (2 L), and extracted with EtOAc. The combined organic layers were washed with water and brine, dried and concentrated to provide 3-bromo-5-fluoro-2-methyl-benzoic acid, which was used directly in the next step.
後処理
- temperaturewarmed to room temperature
- stirringstirred for 16 hrs
- extractionextracted with EtOAc
- washThe combined organic layers were washed with water and brine
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1b7ee77f353746bcaf1d3b5d3002b57a
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09018211B2
反応ノート
読み込み中…