Azobisisobutyronitrile → 1-(Bromomethyl)-3-methoxy-5-methylbenzene

HRID 1066615

反応式

HRID 1066615 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([O:9][CH3:10])[CH:5]=[C:6]([CH3:8])[CH:7]=1.[Br:11]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:11][CH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([O:9][CH3:10])[CH:3]=1

参加物

5

反応物 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 701263,5-Dimethylanisole

生成物 1

HCID 5855341-(Bromomethyl)-3-methoxy-5-methylbenzene収率 68%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A suspension of 3,5-dimethylanisole (13.60 g, 100 mmol), N-bromosuccinimide (18.35 g, 100 mmol) and 2,2′-azobis(2-methylpropionitrile) in CCl4 was heated under reflux for 1 h. The succinimide was filtered off, the filtrate was concentrated and the residue was chromatographed (SiO2, CH2Cl2/hexane 1:4). There were obtained 14.61 g (68%) of 1-bromomethyl-3-methoxy-5-methyl-benzene.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 h
  3. filtrationThe succinimide was filtered off
  4. concentrationthe filtrate was concentrated
  5. customthe residue was chromatographed (SiO2, CH2Cl2/hexane 1:4)

出典と根拠

ORDレコード
ord-10a65cbfb5ea4cdcabe444371a923be5
出典データセット
uspto-grants-2001_06
特許番号
US06242644B1

関連ノート

読み込み中…