Ammonium Chloride → 1-(4-Amino-3-(trifluoromethyl)phenyl)ethanone
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][C:5]=1[C:13]([F:16])([F:15])[F:14])([O-])=O.[NH4+].[Cl-]>CCO.O.[Fe]>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][C:5]=1[C:13]([F:14])([F:15])[F:16]参加物
6
実験手順
A mixture of 1-[4-nitro-3-(trifluoromethyl)phenyl]-1-ethanone (1.41 g, 6.05 mmol), Fe powder (1.69 g, 30.2 mmol), and NH4Cl (324 mg, 6.05 mmol) in EtOH (24 ml) and water (9 ml) was heated to reflux for 2.5 hours. After cooling to room temperature, the mixture was filtered through a pad of Celite and the filtrate was concentrated. And the residue was dissolved with ethyl acetate (100 ml), washed with water (100 ml), dried over MgSO4, and concentrated in vacuo to give 1.22 g (quant.) of the title compound as a pale yellow oil.
後処理
- temperaturewas heated
- temperatureto reflux for 2.5 hours
- filtrationthe mixture was filtered through a pad of Celite
- concentrationthe filtrate was concentrated
- dissolutionAnd the residue was dissolved with ethyl acetate (100 ml)
- washwashed with water (100 ml)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-313ee97aa9c742228677b3d48451b807
- 出典データセット
- uspto-grants-2003_08
- 特許番号
- US06603008B1
反応ノート
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