Benzonitrile, m-chloro- → 3-Chlorobenzamidoxime
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]#[N:6].Cl.[NH2:11][OH:12].[OH-].[Na+]>C(O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:5](=[N:11][OH:12])[NH2:6])[CH:7]=[CH:8][CH:9]=1参加物
6
反応条件
- 温度
- 90 °C
実験手順
A solution of 3.35 mL (30.0 mmol) 3-chlorobenzonitrile in ethanol (40 mL) was added to a solution of 2.47 g (35.5 mmol) hydroxylamine hydrochloride and 1.42 g (35.5 mmol) NaOH in water (20 mL) at r.t. and then heated at 90° C. for 24 h. After cooling, the reaction mixture was concentrated, the residue diluted with water, followed by filtration and drying to afford 1.13 g (93%) of the title compound. 1H NMR: 8.11 (s, 1H), 7.72 (s, 1H), 7.61 (m, 1H), 7.46 (m, 1H), 7.36 (m, 1H).
後処理
- temperatureAfter cooling
- concentrationthe reaction mixture was concentrated
- additionthe residue diluted with water
- filtrationfollowed by filtration
- customdrying
出典と根拠
- ORDレコード
- ord-984eed0d5b914057b9a2f2df9a258a65
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07585881B2
反応ノート
読み込み中…