반응 #1563321

ord-015f3e31eb534fe6b5fcfa39c3a46d91

용매

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted repeatedly with ethyl acetate
  2. 2
    세척The combined organic phases were washed with saturated sodium chloride solution
  3. 3
    건조dried over sodium sulphate
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타The crude product was purified by preparative HPLC

실험 절차

38 mg (0.08 mmol) of methyl-[1-(4-chloro-3-{[(3R)-2-(4-chlorophenyl)-4,4,4-trifluoro-3-methylbutanoyl]amino}phenyl)cyclobutyl]acetate were dissolved in 9.5 ml of dioxane, and 0.15 ml of 1 N aqueous sodium hydroxide solution was added. The mixture was stirred at 80° C. overnight. The reaction mixture was then acidified with 1 N hydrochloric acid to pH 1 and extracted repeatedly with ethyl acetate. The combined organic phases were washed with saturated sodium chloride solution, dried over sodium sulphate and concentrated under reduced pressure. The crude product was purified by preparative HPLC. This gave 22 mg (0.05 mmol, 60% of theory) of the target compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09018414B2uspto-grants-2015_04