反应详情

Into a mixture of 0.5 g (1.6 mmol) of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole-3-carbonitrile, 0.24 g (1.7 mmol) of methyl pyrazinecarboxylate, and 0.5 ml of acetonitrile was gradually added 0.3 g (1.6 mmol) of 28% CH3ONa/CH3OH at room temperature. After 2 hours of stirring at room temperature, 5 ml of water and then concentrated hydrochloric acid were added thereto to make the mixture pH 2, whereby crystals were precipitated. Thereto was added 10 ml of ethyl acetate, followed by extraction. The organic layer was washed with saturated saline and then dried over anhydrous sodium sulfate. After removal of the sodium sulfate by filtration, the layer was concentrated and the resulting crystals were filtrated. The crystals were washed with a small amount of hexane and ethyl acetate and the dried to obtain 0.5 g (yield 77%) of N-[3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole-5-yl]pyrazine-2-carboxamide.

1. customat room temperature
2. customwere precipitated
3. additionThereto was added 10 ml of ethyl acetate
4. extractionfollowed by extraction
5. washThe organic layer was washed with saturated saline
6. dry with materialdried over anhydrous sodium sulfate
7. customAfter removal of the sodium sulfate
8. filtrationby filtration
9. concentrationthe layer was concentrated
10. filtrationthe resulting crystals were filtrated
11. washThe crystals were washed with a small amount of hexane and ethyl acetate
12. customthe dried