Acetyl chloride → 2-Fluoro-4-bromo-4'-acetylbiphenyl

HRID 326961ノート

反応式

HRID 326961 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:7])[CH3:6].[F:9][C:10]1[CH:15]=[C:14]([Br:16])[CH:13]=[CH:12][C:11]=1[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(Cl)Cl>[F:9][C:10]1[CH:15]=[C:14]([Br:16])[CH:13]=[CH:12][C:11]=1[C:17]1[CH:22]=[CH:21][C:20]([C:5](=[O:7])[CH3:6])=[CH:19][CH:18]=1

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 5210634-Bromo-2-fluoro-1,1'-biphenylHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 142048672-Fluoro-4-bromo-4'-acetylbiphenyl

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In a reactor were placed 113 g of anhydrous aluminum chloride and 600 1 of methylene chloride, to which was added 113 g of acetylchloride under stirring at 0° C. or less. Subsequently, a solution of 100 g of 2-fluoro-4-bromobiphenyl in 400 ml methylene chloride was added dropwise, stirred and reacted together for 7 hours while increasing the temperature up to room temperature. After adding the reaction solution to ice/dilute hydrochloric acid, the methylene chloride layer was washed sequentially with water, aqueous sodium hydrogencarbonate solution, and water, followed by dehydration over Glauber's salt and distillation of the solvent. The remaining fraction was recrystallized with acetone to obtain 2-fluoro-4-bromo-4'-acetylbiphenyl.

後処理

  1. customIn a reactor were placed
  2. stirringstirred
  3. customreacted together for 7 hours
  4. additionAfter adding the reaction solution to ice/dilute hydrochloric acid
  5. washthe methylene chloride layer was washed sequentially with water, aqueous sodium hydrogencarbonate solution, and water
  6. distillationfollowed by dehydration over Glauber's salt and distillation of the solvent
  7. customThe remaining fraction was recrystallized with acetone

出典と根拠

ORDレコード
ord-3bd8461ff20c42dd985f0e3ad3590b1f
出典データセット
uspto-grants-1993_12
特許番号
US05271867

反応ノート

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