Reaktion #157761

ord-a2e05521131d48fa887d2bc0d813faf0

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Extraktionfollowed by extraction with ethyl acetate
  2. 2
    WaschenThe organic layer was washed with brine
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    SonstigeThe solvent was then evaporated under reduced pressure
  6. 6
    SonstigeThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:1→0:100)

Vorschrift

Sodium ethanethiolate (2.0 g) was added to a solution of 4-bromo-2-chloro-1-fluorobenzene (5.0 g) in N,N-dimethylformamide (20 mL), and the mixture was stirred at 65° C. for two hours. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:1→0:100) to give the title compound as a colorless oil (4.8 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822503B2uspto-grants-2014_09