Ethanol → Ethyl 2,2-difluoro-1-methylcyclopropane-carboxylate

HRID 248220

Reaktionsgleichung

Reaktionsgleichung von HRID 248220
[F:1][C:2]1([F:9])[CH2:4][C:3]1([CH3:8])[C:5](Cl)=[O:6].[CH2:10]([OH:12])[CH3:11]>S(=O)(=O)(O)O>[F:1][C:2]1([F:9])[CH2:4][C:3]1([CH3:8])[C:5]([O:12][CH2:10][CH3:11])=[O:6]

Komponenten

4

Edukt 2

HCID 702EthanolHCID 146952322,2-Difluoro-1-methylcyclopropane-1-carbonyl chloride

Produkt 1

HCID 14695235Ethyl 2,2-difluoro-1-methylcyclopropane-carboxylateAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidKatalysator

Versuchsvorschrift

35 ml of ethanol are added dropwise at 20° C. to 15.45 g (0.1 mol) of 2,2-difluoro-1-methyl-cyclopropanecarbonyl chloride, with stirring. After the addition of 2 drops of concentrated sulphuric acid, the reaction mixture is refluxed for another hour. Excess ethanol is subsequently distilled off, and the residue is dried and distilled under atmospheric pressure. In this manner, 14.2 g (87% of theory) of ethyl 2,2-difluoro-1-methylcyclopropane-carboxylate are obtained in form of a liquid of boiling point 141°-143° C.

Aufarbeitung

  1. temperaturethe reaction mixture is refluxed for another hour
  2. distillationExcess ethanol is subsequently distilled off
  3. customthe residue is dried
  4. distillationdistilled under atmospheric pressure

Quellen und Nachweise

ORD-Eintrag
ord-2a6031f8ea2b4a4e9ac3f342e3a8cf70
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05208388

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