Ethanol → Fluorodichloromethyl-mercaptomethyl phenyl ketone

HRID 1284842Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1284842
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:3])C.C(O)C.[F:13][C:14](Cl)(Cl)[S:15]Cl.[CH:19]([Cl:22])(Cl)[Cl:20]>>[C:4]1([C:1]([C:14]([F:13])([CH:19]([Cl:22])[Cl:20])[SH:15])=[O:3])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

Komponenten

5

Edukt 4

HCID 702EthanolHCID 6212ChloroformHCID 7410AcetophenoneHCID 759261,1-Dichloro-1-fluoromethanesulfenyl chloride2×

Produkt 1

HCID 86740593Fluorodichloromethyl-mercaptomethyl phenyl ketone

Versuchsvorschrift

240 g (2 moles) of acetophenone were dissolved in 300 ml of chloroform and, after addition of 3 ml of ethanol and 109 g (0.64 mole) of fluorodichloromethanesulphenyl chloride, the mixture was heated to the reflux temperature. A further 400 g (2.36 moles) of fluorodichloromethane-sulphenyl chloride were added dropwise in the course of 30 minutes and the mixture was then heated under reflux for 5 hours. For subsequent working up, the reaction mixture was subjected to fractional distillation under reduced pressure. After first runnings of unchanged starting material, 126 g of fluorodichloromethyl-mercaptomethyl phenyl ketone were obtained in the form of a liquid of boiling point 128° C./0.4 mbar.

Aufarbeitung

  1. temperaturethe mixture was heated to the reflux temperature
  2. temperaturethe mixture was then heated
  3. temperatureunder reflux for 5 hours
  4. distillationthe reaction mixture was subjected to fractional distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a880aca309944014af7832c8d38d1d2f
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04564478

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