반응 #53556

반응 방정식

water

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

cyclobutylmethyl bromide

potassium carbonate

→

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

수율 21.6%

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

0.9 g (3.3 mmol) of 2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile, 0.5 g (3.3 mmol) of cyclobutylmethyl bromide and 0.55 g (4.0 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, 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 by silica gel column chromatography afforded 0.24 g of 2-cyclobutylmethylthio-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 21.2%) as a pale yellow powder (m.p. 102-103° C.).

출처