反応 #1723

反応方程式

sodium chloride

4-ethynylbenzonitrile

2-bromo-5-nitrothiophene

triethylamine

→

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

溶媒

ethyl acetate

dimethylformamide

反応条件

後処理

1. 1
   乾燥The organic layer was dried over anhydrous sodium sulfate
2. 2
   ろ過filtered
3. 3
   その他evaporated to dryness
4. 4
   その他The crude solid was triturated with 1:1 dichloromethane/hexane

実験手順

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.

出典