反応 #80190

ord-15d651bafd9244f8b7ddf9e9319aa1c2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    その他the volatiles were removed under vacuum and 5 ml of water
  3. 3
    workup.ADDITIONwere added to the mixture, which
  4. 4
    抽出The resulting slurry was extracted with ethyl acetate
  5. 5
    乾燥the combined organic layers were dried (magnesium sulfate)
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated under vacuum

実験手順

2-(5-Trifluoromethyl-pyridin-2-yl)-benzoic acid isopropyl ester was dissolved in 10 ml of a 3:1:1 mixture of tetrahydrofuran-methanol-water, and lithium hydroxide monohydrate (161 mg, 3.84 mmol) was added. After stirring for 3 h at room temperature, the volatiles were removed under vacuum and 5 ml of water were added to the mixture, which was brought to pH 6 with 1N HCl. The resulting slurry was extracted with ethyl acetate, the combined organic layers were dried (magnesium sulfate), filtered and concentrated under vacuum to provide the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713489B2uspto-grants-2004_03