反応 #158293

ord-3c8ee0485f7d48f3af8d7a9297adf0a4

溶媒

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    その他the solvent was evaporated under reduced pressure
  3. 3
    その他The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)

実験手順

Under an argon atmosphere, Lawesson's reagent (1.00 g) was added to a suspension of ethyl 3-(3,4-difluorophenyl)-2-oxopiperidine-3-carboxylate (1.00 g) in toluene (20 mL) at room temperature. The reaction mixture was stirred at 110° C. for 4 hr, and allowed to cool to room temperature, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (859 mg).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08822699B2uspto-grants-2014_09