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

HRID 972750笔记

反应方程式

HRID 972750 反应方程式
[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]

参与物

4

反应物 2

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

产物 1

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

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

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##

后处理

  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.)

来源与证据

ORD记录
ord-b2e693431eb244a193848d0f447126be
来源数据集
uspto-grants-1977_10
专利号
US04053616

反应笔记

加载中…