Ammonium Chloride → 3-Bromobenzene-1,2-diamine
反応式
[Br:1][C:2]1[C:3]([N+:9]([O-])=O)=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].[NH4+].[Cl-]>CCO.O.[Fe]>[Br:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:4]([NH2:5])[C:3]=1[NH2:9]参加物
6
実験手順
A mixture of 3-bromo-2-nitroaniline (2 g, 9.2 mmol), Fe powder (1.54 g, 27.6 mmol) and NH4Cl (4.8 g, 52 mmol) in EtOH and H2O was stirred under reflux for 1 h. The mixture was cooled to room temperature and filtered. The filtrate was diluted water extracted with ethyl acetate and the combined organic layers were dried and concentrated in vacuum to give the crude desired product (1.7 g, Yield 85%). This crude was used in the next step without further purification.
後処理
- temperatureunder reflux for 1 h
- filtrationfiltered
- extractionextracted with ethyl acetate
- customthe combined organic layers were dried
- concentrationconcentrated in vacuum
出典と根拠
- ORDレコード
- ord-506ef317dda5490cb76d82cb879053d9
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388173B2
反応ノート
読み込み中…