反応 #1350580

反応方程式

sodium sulfide

2-methyl-4-thiocyanoisophthalonitrile

→

3-Methyl-2,4-dicyanothiophenol

溶媒

water

methanol

water

反応条件

後処理

1. 1
   抽出extracted with methyl tert-butyl ether
2. 2
   抽出the thiophenol was extracted with methylene chloride
3. 3
   洗浄The extract was washed three times with water
4. 4
   その他the organic phase was then separated off
5. 5
   乾燥dried over sodium sulfate
6. 6
   濃縮concentrated

実験手順

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%).

出典