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Azobisisobutyronitrile → HCID 18700114, 화합물

HRID 2289320
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HRID 2289320 반응식
[F:1][C:2]([F:14])([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH3:13])[CH:3]([F:5])[F:4].C1C(=O)N([Br:22])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[F:1][C:2]([F:14])([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][Br:22])[CH:3]([F:4])[F:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 2776650alpha,alpha,beta,beta-Tetrafluoro-2-methylphenetole

생성물 1

HCID 18700114HCID 18700114, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To a stirred solution of 2-(1,1,2,2-tetrafluoroethoxy)toluene (2.5 g, 12.2 mmol) in CCl4 (75 mL) was added NBS (2.1 g, 13 mmol) and AIBN (0.65 g, 3 mmol). The mixture was refluxed for 6 h. The solvent was removed under reduced pressure and the residue was partitioned between EtOAc (75 mL) and water (50 mL). The organic phase was separated, dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by pressurized silica gel column chromatography using hexanes as eluant to give 2-(1,1,2,2-tetrafluoroethoxy)benzyl bromide as a colorless liquid (TLC Rf =0.7 (hexanes)).

후처리

  1. temperatureThe mixture was refluxed for 6 h
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was partitioned between EtOAc (75 mL) and water (50 mL)
  4. customThe organic phase was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent was removed under reduced pressure
  8. customThe residue was purified by pressurized silica gel column chromatography

출처 및 근거

ORD 기록
ord-ab0076abff254452b73db0515c85e17e
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090805

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