反応 #45930

ord-da35513542f84da8825139e72ef6d024

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction was quenched by cold H2O (50 mL)
  2. 2
    抽出the resulting mixture was extracted with EtOAc (3×100 mL)
  3. 3
    洗浄The combined EtOAc extracts were washed with brine (3×50 mL)
  4. 4
    乾燥dried (anhydrous Na2SO4)
  5. 5
    その他The solvent was removed in vacuo

実験手順

To a stirred solution of 6-(3-diethylaminopropoxy)-2,4-difluoronitrobenzene (11 mmol) and triethylamine (22 mmol) in DMF (20 mL), a solution of n-butylamine (11 mmol) in DMF (8 mL) was added dropwise at rt, and the mixture was stirred at rt for 10 h. The reaction was quenched by cold H2O (50 mL), and the resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine (3×50 mL) and dried (anhydrous Na2SO4). The solvent was removed in vacuo to afford the desired 2-n-butylamino-6-(3-diethylaminopropoxy)-4-fluoronitrobenzene which was used for further transformation.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07737285B2uspto-grants-2010_06