Reacción #428831

ord-d4ab15b6213542d2ab6ddd1709c55b24

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction mixture is maintained at 60° C. for 8 hours
  2. 2
    Temperaturacooled to ambient temperature
  3. 3
    ExtracciónThe aqueous phase is extracted with diethyl ether (3×250 ml)
  4. 4
    Lavadowashed with water
  5. 5
    Secadodried over anhydrous sodium sulfate
  6. 6
    FiltraciónThe mixture is filtered
  7. 7
    Otrothe filtrate is evaporated under reduced pressure
  8. 8
    OtroThe residue is purified by column chromatography on silica gel

Procedimiento

A mixture of mercury (II) acetate (7.76 g, 0.024 mol), sulfuric acid (9 ml, 0.09 mol) and water (450 ml) is heated at 60° C. 2-(1,1-dimethylprop-2-ynyloxy)propionic acid methyl ester (90 g, 0.529 mol) is added carefully at 60° C. The reaction mixture is maintained at 60° C. for 8 hours and cooled to ambient temperature. The aqueous phase is extracted with diethyl ether (3×250 ml), the organic phases are combined, washed with water, and dried over anhydrous sodium sulfate. The mixture is filtered, and the filtrate is evaporated under reduced pressure. The residue is purified by column chromatography on silica gel to give 2-(1,1-dimethyl-2-oxopropoxy)propionic acid methyl ester (24 g) as a colorless oil.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08895761B2uspto-grants-2014_11