Nitric Acid → (2-Chloro-5-nitrophenyl)acetonitrile
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]#[N:10].[N+:11]([O-])([OH:13])=[O:12]>ClCCl.OS(O)(=O)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[CH2:8][C:9]#[N:10]参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a solution of 2-chloro-phenyl-acetonitrile (15.0 g, 99.0 mmol) in the dichloromethane (50 mL) and H2SO4 (40 mL) is slowly added a mixture of H2SO4 (14 mL) and HNO3 (5.5 mL) at 0° C. The reaction mixture is stirred at 0° C. for 20 minutes, warmed to room temperature for 30 minutes and then concentrated to remove organic solvent. The solution is poured into a beaker containing ice-water (400 mL) to give a crystalline precipitate, which is collected by vacuum filtration and washed with water to give the title intermediate (13.4 g, 69.0%).
後処理
- temperaturewarmed to room temperature for 30 minutes
- concentrationconcentrated
- customto remove organic solvent
- additionThe solution is poured into a beaker
- additioncontaining ice-water (400 mL)
- customto give a crystalline precipitate, which
- filtrationis collected by vacuum filtration
- washwashed with water
出典と根拠
- ORDレコード
- ord-ded8d23858084359b46e86f8f1efb434
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07449582B2
反応ノート
読み込み中…