Azobisisobutyronitrile → Methyl 2-bromo-2-(3-methoxyphenyl)acetate

HRID 270920노트

반응식

HRID 270920 반응식
CC(N=NC(C#N)(C)C)(C#N)C.[CH3:13][O:14][C:15](=[O:25])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH3:24])[CH:18]=1.C1C(=O)N([Br:33])C(=O)C1>C(Cl)(Cl)(Cl)Cl>[CH3:13][O:14][C:15](=[O:25])[CH:16]([Br:33])[C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH3:24])[CH:18]=1

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 519609Methyl 2-(3-methoxyphenyl)acetate

생성물 1

HCID 289522Methyl 2-bromo-2-(3-methoxyphenyl)acetate

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

AIBN (10 mg) was added to a solution of (3-Methoxy-phenyl)-acetic acid methyl ester (2 g, 11 mmol) in CCl4 (30 ml). The solution was then heated to reflux and NBS (2.3 g, 13 mmol) was added in portions. After complete addition the reaction mixture was refluxed for 4 h. After cooling, solid residue was filtered off and the filtrate concentrated to yield product Bromo-(3-methoxy-phenyl)-acetic acid methyl ester, that was washed repeatedly with pet ether.

후처리

  1. temperatureThe solution was then heated
  2. temperatureto reflux
  3. additionAfter complete addition the reaction mixture
  4. temperaturewas refluxed for 4 h
  5. temperatureAfter cooling
  6. filtrationsolid residue was filtered off
  7. concentrationthe filtrate concentrated

출처 및 근거

ORD 기록
ord-055cd0ad1a504888886fea879d7b9bcb
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449576B1

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