Triethylamine → 2,2,2-Trifluoro-1-(3-nitrophenyl)ethanone oxime
反応式
[F:1][C:2]([F:15])([F:14])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=1)=O.[NH2:16][OH:17].Cl.CCN(CC)CC>CCO>[F:1][C:2]([F:15])([F:14])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=1)=[N:16][OH:17]参加物
5
実験手順
A mixture of 2,2,2-trifluoro-1-(3-nitro-phenyl)ethanone (4 g), NH2OH.HCl (5.037 g), and Et3N (20.44 g) in EtOH (80 mL) was refluxed for 4 days. After concentration, the residue was extracted with CH2Cl2. The organic layer was washed with water and dried over MgSO4. The crude product was purified by silica gel flash chromatography (30% ethyl acetate in hexanes) to give the title compound (3.4 g) as a solid.
後処理
- temperaturewas refluxed for 4 days
- concentrationAfter concentration
- extractionthe residue was extracted with CH2Cl2
- washThe organic layer was washed with water
- dry with materialdried over MgSO4
- customThe crude product was purified by silica gel flash chromatography (30% ethyl acetate in hexanes)
出典と根拠
- ORDレコード
- ord-2278fa11a07f44b9995cb43110b157c1
- 出典データセット
- uspto-grants-2004_12
- 特許番号
- US06831080B2
反応ノート
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