반응 #6115

반응 방정식

3-cyano-4-iodobenzonitrile

sodium thiomethylate

→

expected product

수율 81.0%

3-cyano-4-mercaptobenzonitrile

수율 81.0%

용매

hexamethylphosphoramide

반응 조건

후처리

1. 1
   기타the solution obtained
2. 2
   기타The resulting reaction medium
3. 3
   추출extracted with methylene chloride
4. 4
   세척The organic phase is washed with water
5. 5
   건조dried over magnesium sulfate
6. 6
   기타evaporated under reduced pressure

실험 절차

Under argon, 3.03 g (12.10-3 mol) of 3-cyano-4-iodobenzonitrile and 3.36 g (48.10-3 mol) of sodium thiomethylate are dissolved in 80 ml of anhydrous hexamethylphosphoramide and the solution obtained is then heated at 80° C. for 45 minutes. The resulting reaction medium is hydrolyzed in an ice/1N HCl mixture and then extracted with methylene chloride. The organic phase is washed with water and then dried over magnesium sulfate and evaporated under reduced pressure to give 1.55 g (yield: 81%) of the expected product.

출처