Реакция #586134

Уравнение реакции

water

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

2,2,2-trifluoroethanthiol

potassium carbonate

→

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

Выход 57.1%

Растворители

N,N-dimethylformamide

Условия реакции

Обработка

1. 1
   ДругоеThe resulting reaction mixture
2. 2
   Экстракцияthe organic matters were extracted with 20 ml of ethyl acetate twice
3. 3
   Промывкаwashed with 30 ml of water twice
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
6. 6
   ДругоеPurification of the residue by silica gel column chromatography

Методика

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.).

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