Ammonium Chloride → 1-(3-Amino-5-bromo-2-hydroxyphenyl)ethanone
反応式
[Br:1][C:2]1[CH:3]=[C:4]([N+:12]([O-])=O)[C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.[NH4+].[Cl-]>CCO.O.[Fe]>[NH2:12][C:4]1[C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=[C:2]([Br:1])[CH:3]=1参加物
5
実験手順
A mixture of 1-(5-bromo-2-hydroxy-3-nitrophenyl)ethanone (25 g, 96 mmol), iron (27 g, 481 mmol), and NH4Cl (5.1 g, 96 mmol) in EtOH/H2O (5:1,300 ml) was heated at reflux in 2 h, the mixture was cooled filtered the solid, the filtrate was concentrated, taken up in H2O, extracted with DCM (3×), dried over MgSO4, concentrated and purified by ISCO (10% EtOAc/Hexanes) to give the title compound as a yellow solid. MS (m+2): 232.1.
後処理
- temperaturewas heated
- temperatureat reflux in 2 h
- temperaturethe mixture was cooled
- filtrationfiltered the solid
- concentrationthe filtrate was concentrated
- extractionextracted with DCM (3×)
- dry with materialdried over MgSO4
- concentrationconcentrated
- custompurified by ISCO (10% EtOAc/Hexanes)
出典と根拠
- ORDレコード
- ord-b818bd1d17c44254abff2eb9fb357700
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07951838B2
反応ノート
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