Acetic Acid → 5-Bromo-3-methoxy-2-methylaniline
反応式
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[C:5]([CH3:11])=[C:4]([O:12][CH3:13])[CH:3]=1.C(O)(=O)C>[Fe].C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([O:12][CH3:13])[C:5]([CH3:11])=[C:6]([CH:7]=1)[NH2:8]参加物
5
実験手順
A heterogeneous reaction mixture of 4-bromo-2-methoxy-6-nitrotoluene (500 mg, 2.032 mmol), acetic acid (20 ml), and iron (1135 mg, 20.32 mmol) was stirred at rt for 24 hr. Ethyl acetate was added, then the mixture was filtered through celite and the filtrate concentrated. The residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution. The aqueous layer was extracted with further ethyl acetate. The combined organic phases were washed with water and brine, then dried over sodium sulfate, filtered and concentrated to afford the title compound. MS m/z: 218.0 (M+H)+.
後処理
- filtrationthe mixture was filtered through celite
- concentrationthe filtrate concentrated
- customThe residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution
- extractionThe aqueous layer was extracted with further ethyl acetate
- washThe combined organic phases were washed with water and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-8859f3d5a022483f975f49a9bec80ff7
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09314464B2
反応ノート
読み込み中…