Reaktion #637792

ord-4018fc3a433a476682b6fa34b919530c

Reaktionsbedingungen

Temperatur
65°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture was extracted with dichloromethane (3×)
  2. 2
    WaschenThe organic phase was washed with water (2×), brine
  3. 3
    Trocknendried over sodium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigeevaporated to dryness
  6. 6
    Sonstigeto obtain a crude, which
  7. 7
    Sonstigewas purified by column chromatography on silica gel (exane-EtOAc 9:1)

Vorschrift

A mixture of 2,4-difluoro-benzoic acid tert-butyl ester (30 g, 140.05 mmol) and (S)-2-methoxy-1-methyl-ethylamine (100 mL) was stirred at 65° C. for 2 days. A saturated solution of NaHCO3 was added and the mixture was extracted with dichloromethane (3×). The organic phase was washed with water (2×), brine, dried over sodium sulfate filtered and evaporated to dryness to obtain a crude, which was purified by column chromatography on silica gel (exane-EtOAc 9:1). The title compound (33.38 g, 84%) was obtained as oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07947686B2uspto-grants-2011_05