Chlorodifluoromethane → Ethyl 1,1-diethoxyethyl(difluoromethyl)phosphinate

HRID 729156

Reaktionsgleichung

Reaktionsgleichung von HRID 729156
[H-].[Na+].[CH2:3]([O:5][C:6]([PH:11](=[O:15])[O:12][CH2:13][CH3:14])([O:8][CH2:9][CH3:10])[CH3:7])[CH3:4].Cl[CH:17]([F:19])[F:18]>O1CCCC1>[CH2:9]([O:8][C:6]([P:11]([CH:17]([F:19])[F:18])(=[O:15])[O:12][CH2:13][CH3:14])([O:5][CH2:3][CH3:4])[CH3:7])[CH3:10]

Komponenten

5

Edukt 3

HCID 6372ChlorodifluoromethaneHCID 24758Sodium hydrideHCID 178476820HCID 178476820, Verbindung

Produkt 1

HCID 9992738Ethyl 1,1-diethoxyethyl(difluoromethyl)phosphinate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a suspension of 15.8 g of sodium hydride (dispersion in oil) in 500 ml of tetrahydrofuran are added dropwise 67 g (300 mMol) of ethyl 1,1-diethoxyethylphosphinate at such a rate so that the temperature does not exceed 25° C. This mixture is stirred for one hour at room temperature, then cooled to -10° C. and 77.8 g (900 mMol) of chlorodifluoromethane are introduced. Stirring is continued for another 2 hours at room temperature, then 100 ml of ice-cold water are added. The mixture is extracted three times with dichloromethane and the combined extracts dried over magnesium sulphate. Removal of the solvent in vacuo gives ethyl 1,1-diethoxyethyl(difluoromethyl)phosphinate as a viscous oil,Rf=0.44 (CH2Cl2 /CH3COOH, 9+1).

Aufarbeitung

  1. customdoes not exceed 25° C
  2. temperaturecooled to -10° C.
  3. stirringStirring
  4. waitis continued for another 2 hours at room temperature
  5. extractionThe mixture is extracted three times with dichloromethane
  6. dry with materialthe combined extracts dried over magnesium sulphate
  7. customRemoval of the solvent in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-02fe391efa80496fa3c2b41223b9a2b8
Quelldatensatz
uspto-grants-1991_09
Patentnummer
US05051524

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