반응 #1827700

반응 방정식

4-chlorobenzonitrile

potassium carbonate

water

1-dodecanethiol

→

4-(dodecyl-thio)benzonitrile

수율 96.0%

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   온도is heated
2. 2
   여과The mixture is filtered
3. 3
   세척the filter cake is washed with water
4. 4
   기타The product is recrystallised from methanol
5. 5
   기타dried at 50° C. under vacuum

실험 절차

A suspension consisting of 75.66 g (0.55 mol) of 4-chlorobenzonitrile, 106.42 g (0.77 mol) of potassium carbonate and 111.32 g (0.55 mol) of 1-dodecanethiol is heated, with stirring, under an inert gas atmosphere in 280 ml of N,N-dimethylacetamide to 130° C. and is then stirred at this temperature for 24 hours. After cooling the reaction mixture to room temperature, it is poured on a mixture of 700 g of ice and 750 ml of water. The mixture is filtered and the filter cake is washed with water. The product is recrystallised from methanol and dried at 50° C. under vacuum, affording 160.2 g (96% of theory) of 4-(dodecyl-thio)benzonitrile.

출처