Reacción #6429

ord-32048f4b38654a34b265cba539771b47

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONDuring this addition
  2. 2
    Extracciónis extracted with ether
  3. 3
    Temperaturarefluxed for 20 minutes
  4. 4
    TemperaturaAfter cooling
  5. 5
    Otrothe toluene layer is separated off
  6. 6
    Extracciónthe aqueous phase is extracted with ether in a perforator

Procedimiento

1 mol of 2,3-difluorophenol is dissolved in 1 l of 10% sodium hydroxide solution, and a saturated aqueous solution of 1.1 mol of potassium peroxodisulphate is added dropwise over the course of 4 hours with ice cooling. During this addition, the temperature must not exceed 20o The mixture is stirred overnight at room temperature and neutralized using hydrochloric acid, and unreacted starting material is extracted with ether. 3 1 of toluene and 2 mol of sodium sulphite are added to the aqueous phase, and the mixture is strongly acidified using 1 1 of concentrated hydrochloric acid and refluxed for 20 minutes. After cooling, the toluene layer is separated off, the aqueous phase is extracted with ether in a perforator, and 2,3-difluorohydroquinone is obtained by evaporating the combined toluene and ether extracts.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05248447uspto-grants-1993_09