Reacción #632148

ord-086002285c8e46e786d4b902e6bb00f7

Reactivos

Ninguno

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturacooled in an ice bath
  2. 2
    FiltraciónThe precipitate was filtered
  3. 3
    Lavadowashed twice with ether
  4. 4
    OtroThe filtrate was separated
  5. 5
    Extracciónthe aqueous phase was extracted with ether
  6. 6
    SecadoThe combined ethereal solutions were dried (MgSO4)
  7. 7
    Otroevaporated

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07935704B2uspto-grants-2011_05