Sulfuryl chloride → 1-([1,1′-Biphenyl]-4-yloxy)-1-chloro-3,3-dimethyl-2-butanone

HRID 972750노트

반응식

HRID 972750 반응식
[C:1]1([C:7]2[CH:20]=[CH:19][C:10]([O:11][CH2:12][C:13](=[O:18])[C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(Cl)([Cl:24])(=O)=O>C(Cl)Cl>[Cl:24][CH:12]([O:11][C:10]1[CH:9]=[CH:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:20][CH:19]=1)[C:13](=[O:18])[C:14]([CH3:16])([CH3:17])[CH3:15]

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 230504261-([1,1′-Biphenyl]-4-yloxy)-3,3-dimethyl-2-butanone

생성물 1

HCID 150706801-([1,1′-Biphenyl]-4-yloxy)-1-chloro-3,3-dimethyl-2-butanone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,292 g (4.83 moles) of 1-(4'-phenyl-phenoxy)-3,3-dimethylbutan-2-one were dissolved in 2.5 l of methylene chloride and 400 ml (4.9 moles) of sulfuryl chloride were added dropwise at the boil. The mixture was heated under reflux for 15 hours and was then concentrated by distilling off the solvent. After adding 250 ml of carbon tetrachloride, the solvent was again distilled off under a water-pump vacuum (bath temperature 65° C.). Crude 1-chloro-1-(4'-phenyl-phenoxy)-3,3-dimethylbutan-2-one was obtained quantitatively, and was used further in the form obtained. ##STR3##

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 15 hours
  3. concentrationwas then concentrated
  4. distillationby distilling off the solvent
  5. additionAfter adding 250 ml of carbon tetrachloride
  6. distillationthe solvent was again distilled off under a water-pump vacuum (bath temperature 65° C.)

출처 및 근거

ORD 기록
ord-b2e693431eb244a193848d0f447126be
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04053616

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