反応 #44453

ord-efae84e757614749b3b88bf9a2fe4d09

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The resulting mixture was heated
  2. 2
    温度to reflux
  3. 3
    workup.STIRRINGstirred overnight
  4. 4
    温度at reflux
  5. 5
    抽出followed by extraction with ethyl acetate (3×)
  6. 6
    洗浄The combined organic layers were washed with water and brine
  7. 7
    乾燥dried (Na2SO4)
  8. 8
    その他evaporated

実験手順

Cs2CO3 (4 g, 12.3 mmol) was added to a solution of phenol (1 g, 10.6 mmol) in 50 mL of THF under N2 atmosphere. After stirring for 15 min. 1,4-dibromo-2-nitrobenzene (2.81 g, 10 mmol) was added. The resulting mixture was heated to reflux and stirred overnight at reflux. Water and ethyl acetate were added, followed by extraction with ethyl acetate (3×). The combined organic layers were washed with water and brine, dried (Na2SO4) and evaporated to give the crude compound (3.2 g, 75%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07737136B2uspto-grants-2010_06