Azobisisobutyronitrile → 2-(1-Naphthyl)benzyl bromide

HRID 1006078

反応式

HRID 1006078 の反応式
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:17])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[Br:18]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH2:17][Br:18])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 3016790(Methylphenyl)naphthalene

生成物 1

HCID 110773332-(1-Naphthyl)benzyl bromide

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

114 g (0.52 mol) of 6 and 103 g (0.58 mol) of N-bromosuccinimide were dissolved at room temperature in 2000 cm3 of carbon tetrachloride, admixed with 3 g of azobisisobutyronitrile and heated under reflux for 4 hours. The precipitated succinimide was filtered off, the solvent was removed under reduced pressure and the residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1). This gave 141 g (82%) of 7 as a colorless lacrymatory oil.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 4 hours
  3. filtrationThe precipitated succinimide was filtered off
  4. customthe solvent was removed under reduced pressure
  5. filtrationthe residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1)

出典と根拠

ORDレコード
ord-b4533589758848d5800a1f21321438fe
出典データセット
uspto-grants-2004_09
特許番号
US06787618B1

関連ノート

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