反应 #586126

反应方程式

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

Rongalite

potassium carbonate

2,2,2-trifluoroethyl iodide

→

2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzonitrile

收率 142.3%

溶剂

water

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他The resulting reaction mixture
2. 2
   萃取extracted with 50 ml of ethyl acetate twice
3. 3
   洗涤The ethyl acetate layer was washed with 50 ml of water twice
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
6. 6
   其他Purification of the residue by silica gel column chromatography

实验过程

2.7 g (5.0 mmol) of 1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene], 3.0 g (19.5 mmol) of Rongalite, 3.0 g (21.7 mmol) of potassium carbonate and 6.1 g (29.0 mmol) of 2,2,2-trifluoroethyl iodide were stirred in 50 ml of N,N-dimethylformamide at room temperature for 3 hours. The resulting reaction mixture was poured into 300 ml of water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 2.5 g of 2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 71.4%) as a brown solid (m.p. 65-67° C.).

来源