4-Chlorophenol → 1-(p-Chlorophenoxy)-3,3-dimethyl-4-chloro-2-butanone

HRID 127236

反応式

HRID 127236 の反応式
Br[CH2:2][C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][Cl:6].[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:6][CH2:5][C:4]([CH3:8])([CH3:7])[C:3](=[O:9])[CH2:2][O:17][C:14]1[CH:15]=[CH:16][C:11]([Cl:10])=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 46844-ChlorophenolHCID 11430Potassium CarbonateHCID 104207672-Butanone, 1-bromo-4-chloro-3,3-dimethyl-

生成物 1

HCID 201382951-(p-Chlorophenoxy)-3,3-dimethyl-4-chloro-2-butanone収率 80.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

213 g (1 mol) of 1-bromo-4-chloro-3,3-dimethyl-butan-2-one were added dropwise to a boiling suspension of 128.5 g (1 mol) of 4-chlorophenol and 140 g (1 mol) of potassium carbonate in 1,000 ml of absolute acetone. The mixture was stirred for 15 hours under reflux and was then allowed to cool, and the inorganic residue was filtered off and rinsed with acetone. The filtrate was concentrated by distilling off the solvent in vacuo and the residue was taken up in 1,000 ml of methylene chloride, washed three times with 250 ml of water at a time, dried over sodium sulphate and distilled. 210 g (80.7% of theory) of 4-chloro-1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one of boiling point 125°-127° C./0.1 mm Hg were obtained.

後処理

  1. temperatureunder reflux
  2. temperatureto cool
  3. filtrationthe inorganic residue was filtered off
  4. washrinsed with acetone
  5. concentrationThe filtrate was concentrated
  6. distillationby distilling off the solvent in vacuo
  7. washwashed three times with 250 ml of water at a time
  8. dry with materialdried over sodium sulphate
  9. distillationdistilled

出典と根拠

ORDレコード
ord-d5fa27dfe783477ba495ec12cf37b38e
出典データセット
uspto-grants-1981_03
特許番号
US04255434

関連ノート

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