反应 #1350580

反应方程式

sodium sulfide

2-methyl-4-thiocyanoisophthalonitrile

→

3-Methyl-2,4-dicyanothiophenol

溶剂

water

methanol

water

反应条件

后处理

1. 1
   萃取extracted with methyl tert-butyl ether
2. 2
   萃取the thiophenol was extracted with methylene chloride
3. 3
   洗涤The extract was washed three times with water
4. 4
   其他the organic phase was then separated off
5. 5
   干燥dried over sodium sulfate
6. 6
   浓缩concentrated

实验过程

At 25-35° C., a solution of 110.5 g (0.85 mol) of 60 percent pure sodium sulfide in 425 ml of water was added dropwise to a solution of 170 g (0.85 mol) of 2-methyl-4-thiocyanoisophthalonitrile in 850 ml of methanol, and the mixture was stirred at room temperature for 3 hours. The mixture was then admixed with 1000 ml of water and extracted with methyl tert-butyl ether. The aqueous phase was acidified to pH 1 using HCl, and the thiophenol was extracted with methylene chloride. The extract was washed three times with water, and the organic phase was then separated off, dried over sodium sulfate and concentrated. Yield: 150 g (99%).

来源