Nitric Acid → (2-Chloro-5-nitrophenyl)acetonitrile

HRID 270710

反応式

HRID 270710 の反応式
[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

反応物 2

HCID 944Nitric AcidHCID 76112(o-Chlorophenyl)acetonitrile

生成物 1

HCID 53396322(2-Chloro-5-nitrophenyl)acetonitrile収率 69%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid溶媒2 回HCID 6344Dichloromethane溶媒

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

  1. temperaturewarmed to room temperature for 30 minutes
  2. concentrationconcentrated
  3. customto remove organic solvent
  4. additionThe solution is poured into a beaker
  5. additioncontaining ice-water (400 mL)
  6. customto give a crystalline precipitate, which
  7. filtrationis collected by vacuum filtration
  8. 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

関連ノート

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