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

HRID 127236

반응식

HRID 127236 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d5fa27dfe783477ba495ec12cf37b38e
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255434

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