反応 #586134

反応方程式

water

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

2,2,2-trifluoroethanthiol

potassium carbonate

→

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

収率 57.1%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   抽出the organic matters were extracted with 20 ml of ethyl acetate twice
3. 3
   洗浄washed with 30 ml of water twice
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
6. 6
   その他Purification of the residue by silica gel column chromatography

実験手順

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.).

出典