反应 #586148

反应方程式

2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile

water

→

1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene]

收率 46.4%

溶剂

dimethyl sulfoxide

反应条件

后处理

1. 1
   萃取the organic matters were extracted with 20 ml of ethyl acetate twice
2. 2
   洗涤washed with 30 ml of water twice
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
5. 5
   其他Purification of the residue

实验过程

3.0 g (11.1 mmol) of 2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile in 5 ml of dimethyl sulfoxide was stirred at 50° C. for 2 hours. The reaction mixture was cooled to room temperature and poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, then washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue afforded 1.3 g of 1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene] (yield 42.4%) as a yellow solid, which was used in Example 2 (3) as the starting material.

来源