반응 #357873

ord-5cef8f316395478d8ffe4cffcc609f28

반응 방정식

N#CCc1c(Cl)cccc1Cl
2,6-dichloro-phenyl-acetonitrile
O=[N+]([O-])O
HNO3
N#CCc1c(Cl)ccc([N+](=O)[O-])c1Cl
product
수율 82.4%
N#CCc1c(Cl)ccc([N+](=O)[O-])c1Cl
2,6-dichloro-3-nitrophenyl-acetonitrile
수율 82.4%

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITwarned to room temperature for half hour
  2. 2
    농축concentrated
  3. 3
    기타to remove organic solvent
  4. 4
    workup.ADDITIONThe solution is poured into a beaker
  5. 5
    workup.ADDITIONcontaining ice-water (400 mL)
  6. 6
    기타to give a crystalline precipitate, which
  7. 7
    여과is collected by vacuum filtration
  8. 8
    세척washed with water

실험 절차

To a solution of 2,6-dichloro-phenyl-acetonitrile (15.0 g, 80.62 mmol) in the dichloromethane (50 mL) and H2SO4 (40 mL) is added (slowly) 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, warned to room temperature for half hour, 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 afford the product (20.44 g, 82.4%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07449582B2uspto-grants-2008_11