反应 #44453

ord-efae84e757614749b3b88bf9a2fe4d09

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  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
    萃取followed by extraction with ethyl acetate (3×)
  6. 6
    洗涤The combined organic layers were washed with water and brine
  7. 7
    干燥dried (Na2SO4)
  8. 8
    其他evaporated

实验过程

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%).

来源

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