반응 #586134

반응 방정식

water

2-chloro-4-(4-trifluoromethylpyrazolyl)benzonitrile

2,2,2-trifluoroethanthiol

potassium carbonate

→

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

수율 57.1%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   추출the organic matters were extracted with 20 ml of ethyl acetate twice
3. 3
   세척washed with 30 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

0.65 g (2.4 mmol) of 2-chloro-4-(4-trifluoromethylpyrazolyl)benzonitrile, 0.33 g (2.9 mmol) of 2,2,2-trifluoroethanthiol and 0.40 g (2.9 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at room temperature overnight. The resulting reaction mixture was 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, 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 by silica gel column chromatography afforded 0.48 g of 2-(2,2,2-trifluoroethylthio)-4-(4-trifluoromethylpyrazolyl)benzonitrile (yield 57.1%) as a milk-white powder (m.p. 90-91° C.).

출처