反应 #1723

ord-f537d62089cd4cba9bc833054c2f705b

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    干燥The organic layer was dried over anhydrous sodium sulfate
  2. 2
    过滤filtered
  3. 3
    其他evaporated to dryness
  4. 4
    其他The crude solid was triturated with 1:1 dichloromethane/hexane

实验过程

To a solution of 4-ethynylbenzonitrile (0.5 g), 2-bromo-5-nitrothiophene (0.9 g) and bis(triphenylphosphine)palladium dichloride (83 mg) in anhydrous dimethylformamide (4 ml) was added triethylamine (2.2 ml). The reaction mixture was stirred at room temperature for 3 days then ethyl acetate (200 ml) and saturated sodium chloride (200 ml) were added. The organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to dryness. The crude solid was triturated with 1:1 dichloromethane/hexane followed by diethyl ether to give 4-[(5-nitro-2-thienyl)ethynyl]benzonitrile as a yellow solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726195uspto-grants-1998_03