반응 #586132

반응 방정식

4-(5-trifluoromethylpyridin-2-yl)-2-fluorobenzonitrile

S-cyclopropylmethylisothiourea hydrobromide salt

sodium hydroxide

→

2-cyclopropylmethylthio-4-(5-trifluoromethylpyridin-2-yl)benzonitrile

수율 96.8%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
2. 2
   기타the reaction mixture was separated with 50 ml of water and 50 ml of ethyl acetate
3. 3
   세척The organic layer was washed with 50 ml of water twice
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

실험 절차

1.8 g (6.8 mmol) of 4-(5-trifluoromethylpyridin-2-yl)-2-fluorobenzonitrile, 1.6 g (7.6 mmol) of S-cyclopropylmethylisothiourea hydrobromide salt and 50 ml of N,N-dimethylformamide were put into a round-bottomed flask and stirred together with 1.6 g (8 mmol) of 20% aqueous sodium hydroxide overnight. The solvent was distilled off under reduced pressure, and the reaction mixture was separated with 50 ml of water and 50 ml of ethyl acetate. The organic layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 2.2 g of 2-cyclopropylmethylthio-4-(5-trifluoromethylpyridin-2-yl)benzonitrile (yield 96%) as pale yellow feathery crystals (m.p. 135-136° C.).

출처