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Hydrofluoric Acid → 1-Chloro-1,2,2,2-tetrafluoroethylthiobenzene

HRID 4741
ノート
印刷プレビュー

反応式

HRID 4741 の反応式
[Cl:1][C:2]1(Cl)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]1[S:8][CH2:9][C:10]([F:13])([F:12])[F:11].[FH:15].[Sb](Cl)(Cl)(Cl)(Cl)Cl>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][CH:9]([F:15])[C:10]([F:13])([F:12])[F:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 14917Hydrofluoric AcidHCID 24294Antimony pentachlorideHCID 704105191,1-Dichloro-2,2,2-trifluoroethylthiobenzene

生成物 1

HCID 201518931-Chloro-1,2,2,2-tetrafluoroethylthiobenzene

実験手順

A 500 ml polytetrafluoroethylene reactor equipped with stirrer, thermometer and reflux condenser is charged with 24.7 g (0.094 mol) of 1,1-dichloro-2,2,2-trifluoroethylthiobenzene which are subsequently condensed with 50 g of hydrogen fluoride. 4.2 g (0.014 mol; corresponding to 15 mol%) of antimony pentachloride are added at a temperature of 20° C. The resultant hydrogen chloride is removed from the reactor through the reflux condenser. After 3 hours a further 1.4 g (5 mol%) and after 4 hours a further 2.8 g (10 mol%) of antimony pentachloride are added. After a total reaction time of 5 hours, the hydrogen fluoride is removed by distillation, the residue is dissolved in 150 ml of methylene chloride and the solution is extracted with water. The solution is separated by distillation, affording 1-chloro-1,2,2,2-tetrafluoroethylthiobenzene. Boiling point 178°-179° C., nD20 =1.4732.

後処理

  1. customA 500 ml polytetrafluoroethylene reactor equipped with stirrer
  2. temperaturethermometer and reflux condenser
  3. customThe resultant hydrogen chloride is removed from the reactor through the reflux condenser
  4. additionafter 4 hours a further 2.8 g (10 mol%) of antimony pentachloride are added
  5. customAfter a total reaction time of 5 hours, the hydrogen fluoride is removed by distillation
  6. dissolutionthe residue is dissolved in 150 ml of methylene chloride
  7. extractionthe solution is extracted with water
  8. customThe solution is separated by distillation

出典と根拠

ORDレコード
ord-53a85923a86c4172acc0fb7d8d5d8d30
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04727187

反応ノート

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