반응 #1723

반응 방정식

sodium chloride

4-ethynylbenzonitrile

2-bromo-5-nitrothiophene

triethylamine

→

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

용매

ethyl acetate

dimethylformamide

반응 조건

후처리

1. 1
   건조The organic layer was dried over anhydrous sodium sulfate
2. 2
   여과filtered
3. 3
   기타evaporated to dryness
4. 4
   기타The crude solid was triturated with 1:1 dichloromethane/hexane

실험 절차

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.

출처