Chloroform → Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

HRID 5170

Reaktionsgleichung

Reaktionsgleichung von HRID 5170
C[Si]([PH:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])([O-:9])[O:6][CH2:7][CH3:8])(C)C.[CH:17]([C:19]([CH3:21])=[O:20])=[CH2:18].C(Cl)(Cl)Cl>O>[O:20]=[C:19]([CH3:21])[CH2:17][CH2:18][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8]

Komponenten

5

Edukt 3

HCID 6212ChloroformHCID 6570Methyl vinyl ketoneHCID 178418659HCID 178418659, Verbindung

Produkt 1

HCID 14362820Ethyl 3-oxobutyl(diethoxymethyl)phosphinate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

15.0 g of ethyl trimethylsilyl(diethoxymethyl)phosphonite are added dropwise to a stirred solution of 3.9 g of methyl vinyl ketone under an atmosphere of nitrogen at room temperature. The mixture is then heated to 50° C. for a period of 1 hour. The mixture is then allowed to cool to room temperature, 25 ml of chloroform is then added followed by 10 ml water and this mixture is vigorously stirred for a period of 0.5 h. The organic layer is then separated, dried over magnesium sulphate and concentrated under reduced pressure and the crude product distilled under reduced pressure to give ethyl 3-oxobutyl(diethoxymethyl)phosphinate, b.p. 130°-135° C./0.02 mbar, 31P=+45.3 ppm (CDCl3).

Aufarbeitung

  1. temperatureto cool to room temperature
  2. customThe organic layer is then separated
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated under reduced pressure
  5. distillationthe crude product distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-30eae213606d47d0a395349b420efeef
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05243062

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