Reaktion #89566

ord-27a53808ec9247f3be64a0dcdee0caad

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 4 h
  2. 2
    Einengenconcentrated to half volume under reduced pressure
  3. 3
    Extraktionextracted with EtOAc
  4. 4
    TrocknenThe combined extracts were dried over anhydrous Na2SO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated under reduced pressure
  7. 7
    SonstigeThe residue was dried under high vacuum

Vorschrift

A solution of methyl 2,3-difluoro-6-(pyrimidin-2-yl)benzoate in 2 N NaOH and water was heated at reflux for 4 h. After this time, the reaction mixture was cooled to rt and concentrated to half volume under reduced pressure. The resulting mixture was acidified to pH 4 with 1 N HCl and extracted with EtOAc. The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was dried under high vacuum to give the title compound. ESI MS (M+H) 237.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440982B2uspto-grants-2016_09