反応 #11759

ord-24de28c01492459da7718205e54db758

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction was refluxed for 4 hours
  2. 2
    温度cooled
  3. 3
    洗浄washed with brine
  4. 4
    その他The organic layer was separated
  5. 5
    乾燥dried over magnesium sulfate
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated in vacuo

実験手順

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.29 g, 0.96 mmol) in 2-butanone (10 mL) was added 5-chloro-2-hydroxy-benzenesulfonamide (0.20 g, 0.96 mmol), potassium carbonate (0.27 g, 1.92 mmol) and potassium iodide (0.16 g, 0.96 mmol). The reaction was refluxed for 4 hours, cooled diluted with ethyl acetate and washed with brine. The organic layer was separated, dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (0.32 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098212B2uspto-grants-2006_08