反応 #72917

ord-07072eefa89c499998446616e2b2cd7c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with dichloromethane
  2. 2
    洗浄The organic layer was washed with water and brine
  3. 3
    乾燥dried over Na2SO4
  4. 4
    その他evaporated
  5. 5
    その他Purification by flash chromatography (eluant dichloromethane/methanol 7/3)

実験手順

A solution of 800 mg (5.67 mmol) of 1-fluoro-4-nitrobenzene, 2.07 g (1.2 mmol) of 1-tert-butylpiperazine dihydrobromide and 3.2 mL (20.41 mmol) of triethylamine, in 22 mL of acetonitrile, was refluxed for 10 hours. The mixture was cooled to room temperature, diluted with water and extracted with dichloromethane. The organic layer was washed with water and brine, dried over Na2SO4 and evaporated. Purification by flash chromatography (eluant dichloromethane/methanol 7/3) yielded 860 mg of the title compound as yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541429B2uspto-grants-2013_09