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

HRID 270710

반응식

HRID 270710 반응식
[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]

참가 물질

5

반응물 2

HCID 944Nitric AcidHCID 76112(o-Chlorophenyl)acetonitrile

생성물 1

HCID 53396322(2-Chloro-5-nitrophenyl)acetonitrile수율 69%

시약·촉매·용매 2

HCID 1118Sulfuric Acid용매2회HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ded8d23858084359b46e86f8f1efb434
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449582B2

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