Reaktion #1179916

ord-e975758c79c64f1bac8404f5b47ef947

Reaktionsgleichung

C[CH2][K].O=C(O)CC(=O)O
Ethyl potassium malonate
Cl
HCl
CCOC(=O)CC(=O)O
monoethyl hydrogen malonate
Ausbeute 99.0%

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled in an ice bath
  2. 2
    FiltrationThe precipitate was filtered
  3. 3
    Waschenwashed twice with ether
  4. 4
    SonstigeThe filtrate was separated
  5. 5
    Extraktionthe aqueous phase was extracted with ether
  6. 6
    TrocknenThe combined ethereal solutions were dried (MgSO4)
  7. 7
    Sonstigeevaporated

Vorschrift

Ethyl potassium malonate (25.0 g, 0.15 mol) was suspended in water (15.6 ml) and cooled in an ice bath. Concentrated HCl (12.5 ml) was added dropwise over 30 min, then the mixture was stirred for a further 10 min. The precipitate was filtered, then washed twice with ether. The filtrate was separated and the aqueous phase was extracted with ether. The combined ethereal solutions were dried (MgSO4) and evaporated to afford, as an oil, monoethyl hydrogen malonate (19.2 g, 99%) which was dried under vacuum overnight (or 50°/1 mm for 1 h) prior to use.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08129527B2uspto-grants-2012_03