反应详情

0.76 g of 1-(chloromethyl)-1H-pyrazole hydrochloride and 0.81 g of (3,3,3-trifluoropropyl)malononitrile were dissolved in 10 ml of N,N-dimethylformamide. 1.38 g of potassium carbonate was added to the solution under ice cooling with stirring, followed by stirring at room temperature for 5 hours. Water was added to the reaction mixture, and then extracted with methyl-t-butyl ether (may be referred as MTBE, hereinafter) . The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was recrystallized from hexane-ethyl acetate to obtain 0.36 g of (1H-pyrazole-1-yl methyl) (3,3,3-trifluoropropyl) malononitrile (referred as the compound of the present invention (1), hereinafter) shown by below formula.

1. stirringby stirring at room temperature for 5 hours
2. extractionextracted with methyl-t-butyl ether (
3. washThe organic layer was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was recrystallized from hexane-ethyl acetate