반응 #53563

반응 방정식

water

3-trifluoromethyl-1H-triazol

4-chloro-2-n-propylthiobenzonitrile

potassium carbonate

→

2-propylthio-4-(3-trifluoromethyl-1H-triazolyl)benzonitrile

수율 38.2%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   추출the organic matters were extracted with 50 ml of ethyl acetate twice
3. 3
   세척washed with 50 ml of water twice
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
6. 6
   기타Purification of the residue by silica gel column chromatography

실험 절차

1.06 g (7.7 mmol) of 3-trifluoromethyl-1H-triazol, 1.38 g (6.5 mmol) of 4-chloro-2-n-propylthiobenzonitrile and 1.07 g (7.7 mmol) of potassium carbonate were stirred in 10 ml of N,N-dimethylformamide at 150° C. for 2 hours. The resulting reaction mixture was cooled to the room temperature and poured into 100 ml of water, and the organic matters were extracted with 50 ml of ethyl acetate twice. The ethyl acetate layers were combined, then washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 0.78 g of 2-propylthio-4-(3-trifluoromethyl-1H-triazolyl)benzonitrile. (yield 38.2%) as a milk-white powder (m.p. 143-144° C.).

출처