Reacción #1869219

ord-f3955082ebdf49f99c8913127af764d7

Disolventes

Condiciones de reacción

Temperatura
80°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe resulting mixture was cooled
  2. 2
    FiltraciónSolid (bis-alkylated product) was filtered off
  3. 3
    Extracciónwas extracted with ether
  4. 4
    Otrothe organics were dried
  5. 5
    Concentraciónconcentrated in vacuo
  6. 6
    OtroPurification by RPHPLC (Xterra, gradient 95-5%, ammonia (0.2% aq.) in acetonitrile)

Procedimiento

A mixture of 4,6-dichlororesorcinol (2 g), potassium carbonate (1.54 g) and methyl bromoacetate (1.71 g) in DMF (10 ml) was heated at 80° C. for 24 h. The resulting mixture was cooled and water (200 ml) added. Solid (bis-alkylated product) was filtered off, then the aqueous was acidified with aq. HCl, which was extracted with ether and the organics were dried and concentrated in vacuo. Purification by RPHPLC (Xterra, gradient 95-5%, ammonia (0.2% aq.) in acetonitrile) gave the subtitle compound (0.65 g) as a solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07498338B2uspto-grants-2009_03