반응 #586126

반응 방정식

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

수율 142.3%

용매

water

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   추출extracted with 50 ml of ethyl acetate twice
3. 3
   세척The ethyl acetate layer was washed with 50 ml of water twice
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
6. 6
   기타Purification of the residue by silica gel column chromatography

실험 절차

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.).

출처