Methanol → Methyl 3-bromobenzoate
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[CH3:11]O>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:7][CH3:11])=[O:6]参加物
4
実験手順
Part A: 3-Bromobenzoic acid (1.1 g, 5.47 mmol) was dissolved in methanol (20 ml) in a 50 ml flask. Concentrated sulfuric acid (2 drops) was added and the mixture was refluxed under nitrogen for ten hours then concentrated under reduced pressure. The residue was mixed with dichloromethane (20 ml) and saturated sodium bicarbonate solution (10 ml). The organic material was separated, dried (MgSO4) and concentrated under reduced pressure. The residue was flushed through silica gel with hexane/ethyl acetate (3:1), and concentrated which provided methyl 3-bromobenzoate (1.0 g, 85%).
後処理
- temperaturethe mixture was refluxed under nitrogen for ten hours
- concentrationthen concentrated under reduced pressure
- additionThe residue was mixed with dichloromethane (20 ml) and saturated sodium bicarbonate solution (10 ml)
- customThe organic material was separated
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
- customThe residue was flushed through silica gel with hexane/ethyl acetate (3:1)
- concentrationconcentrated which
出典と根拠
- ORDレコード
- ord-02beae4f681d488aae48056e2215c553
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05622937
反応ノート
読み込み中…