反应 #1722

反应方程式

2-bromo-5-nitrofuran

triethylamine

4-Ethynylbenzonitrile

→

4-[(5-nitro-2-furyl)-ethynyl]benzonitrile

溶剂

acetonitrile

反应条件

后处理

1. 1
   其他The mixture was evaporated to dryness
2. 2
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane (200 ml)
3. 3
   干燥dried over anhydrous sodium sulfate
4. 4
   过滤filtered
5. 5
   其他evaporated to dryness
6. 6
   其他The residue was purified by silica gel chromatography (ethyl acetate/hexane 1:10)
7. 7
   其他triturated with ethyl acetate/hexane (1:3)

实验过程

To a solution of 2-bromo-5-nitrofuran (1.65 g) and triethylamine (34 ml) in anhydrous acetonitrile (55 ml) under nitrogen was added bis(triphenylphosphine)palladium dichloride (130 mg) and cuprous iodide (35 mg). 4-Ethynylbenzonitrile (1.09 g) was added and the reaction mixture was stirred under nitrogen overnight. The mixture was evaporated to dryness and the residue was dissolved in dichloromethane (200 ml), dried over anhydrous sodium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel chromatography (ethyl acetate/hexane 1:10) and triturated with ethyl acetate/hexane (1:3) to give 4-[(5-nitro-2-furyl)-ethynyl]benzonitrile.

来源