反応 #6115

反応方程式

3-cyano-4-iodobenzonitrile

sodium thiomethylate

→

expected product

収率 81.0%

3-cyano-4-mercaptobenzonitrile

収率 81.0%

溶媒

hexamethylphosphoramide

反応条件

後処理

1. 1
   その他the solution obtained
2. 2
   その他The resulting reaction medium
3. 3
   抽出extracted with methylene chloride
4. 4
   洗浄The organic phase is washed with water
5. 5
   乾燥dried over magnesium sulfate
6. 6
   その他evaporated under reduced pressure

実験手順

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.

出典