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

HRID 326961

반응식

HRID 326961 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3bd8461ff20c42dd985f0e3ad3590b1f
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05271867

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