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

HRID 972750ノート

反応式

HRID 972750 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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##

後処理

  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.)

出典と根拠

ORDレコード
ord-b2e693431eb244a193848d0f447126be
出典データセット
uspto-grants-1977_10
特許番号
US04053616

反応ノート

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