1,2-Dichloroethane → 1-(4'-Bromo(1,1'-biphenyl)-4-yl)ethan-1-one

HRID 251770

反応式

HRID 251770 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].ClCCCl.[C:9](Cl)(=[O:11])[CH3:10].[Br:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:16][CH:15]=1>O>[Br:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[CH:25]=[CH:24][C:23]([C:9](=[O:11])[CH3:10])=[CH:22][CH:21]=2)=[CH:18][CH:19]=1

参加物

6

反応物 4

HCID 111,2-Dichloroethane2 回HCID 6367Acetyl chlorideHCID 71014-BromobiphenylHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 798061-(4'-Bromo(1,1'-biphenyl)-4-yl)ethan-1-one収率 102.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Four point three grams (32 mmol) of aluminum chloride was placed into 30 milliliter of 1,2-dichloroethane and a solution made by dissolving 2.0 g (25 mmol) of acetyl chloride, subsequently 5.0 g (21 mmol) of 4-bromo biphenyl into 20 milliliter of 1,2-dichloroethane was added while cooling with ice. The mixed solution was stirred as it is while cooling with ice for 4 hours. After completion of the reaction, adding water and an extraction was carried out using dichloro-methane. Further, washing with water, dried with the use of sodium sulfate. Removing the solvent by distillation, 5.9 g of crude 1-(4′-bromo-biphenyl-4-yl)-ethanone was obtained.

後処理

  1. additionwas added
  2. temperaturewhile cooling with ice
  3. temperaturewhile cooling with ice for 4 hours
  4. customAfter completion of the reaction
  5. extractionan extraction
  6. washFurther, washing with water
  7. dry with materialdried with the use of sodium sulfate
  8. customRemoving the solvent
  9. distillationby distillation

出典と根拠

ORDレコード
ord-77e2e9fe06a04dd18e6c45b442fccbf2
出典データセット
uspto-grants-2011_01
特許番号
US07867629B2

関連ノート

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