(NE)-N-[(5-bromo-2-fluoro-3-methylphenyl)methylidene]hydroxylamine → 5-Bromo-2-fluoro-3-methyl-benzonitrile
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH3:12])[C:5]([F:11])=[C:6]([CH:10]=1)/[CH:7]=[N:8]/O>C(OC(=O)C)(=O)C.O>[Br:1][C:2]1[CH:3]=[C:4]([CH3:12])[C:5]([F:11])=[C:6]([CH:10]=1)[C:7]#[N:8]参加物
4
実験手順
A stirred solution of (E)-5-bromo-2-fluoro-3-methylbenzaldehyde oxime (0.5 g, 2.2 mmol) in acetic anhydride (5.0 mL) was heated to reflux for 18 h. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined ethyl acetate layer was washed with brine and dried over Na2SO4 and concentrated under reduced pressure to afford the crude compound as a light brown gummy material (0.4 g, crude): ESIMS m/z 213.82 ([M+H]+).
後処理
- temperatureto reflux for 18 h
- extractionextracted with ethyl acetate
- washThe combined ethyl acetate layer was washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-87efe7e498914b599e71f32e2a83f8e8
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09211281B2
反応ノート
読み込み中…