반응 #89566

ord-27a53808ec9247f3be64a0dcdee0caad

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 4 h
  2. 2
    농축concentrated to half volume under reduced pressure
  3. 3
    추출extracted with EtOAc
  4. 4
    건조The combined extracts were dried over anhydrous Na2SO4
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure
  7. 7
    기타The residue was dried under high vacuum

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440982B2uspto-grants-2016_09