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

HRID 270920ノート

反応式

HRID 270920 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-055cd0ad1a504888886fea879d7b9bcb
出典データセット
uspto-grants-2008_11
特許番号
US07449576B1

反応ノート

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