Benzoyl Peroxide → 1-Bromo-2-(bromomethyl)-3-methylbenzene

HRID 427513

反応式

HRID 427513 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[CH3:9].[Br:10]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>ClC(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[CH2:9][Br:10]

参加物

5

反応物 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 684723-Bromo-o-xylene

生成物 1

HCID 133583181-Bromo-2-(bromomethyl)-3-methylbenzene収率 45%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A mixture of 3-bromo-o-xylene (15 g, 81 mmol), N-bromo succinimid (15.1 g, 85.1 mmol), dibenzoylperoxid (0.65 g) and tetrachloromethane (150 ml) was refluxed for 5 hours. After filtration the filtrate was washed with sodium hydrogensulfite and water. The organic layer was dried over sodium sulfate and evaporated in vacuo. Chromatography (SiO2) (petroleum ether:ethyl acetate, 100:4) gave a 16.8 g fraction of a mixture containing 45% of the title compound. This mixture was used without further purification.

後処理

  1. temperaturewas refluxed for 5 hours
  2. filtrationAfter filtration the filtrate
  3. washwas washed with sodium hydrogensulfite and water
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customevaporated in vacuo
  6. customChromatography (SiO2) (petroleum ether:ethyl acetate, 100:4) gave a 16.8 g fraction of a mixture

出典と根拠

ORDレコード
ord-51db4384e25a49baa3d78657a3dfbb95
出典データセット
uspto-grants-2001_11
特許番号
US06313137B1

関連ノート

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