反应详情

0.24 g of potassium peroxodisulfate and 0.02 g of sulfuric acid were added to a N,N-dimethylformamide 3 ml solution comprising 0.10 g of 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxamide, followed by reflux with heating. 1.5 hours later, the reaction liquid was stood to cool and poured to 10 ml of water, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 1/2) to obtain 0.09 g of the desired product.

1. temperatureby reflux
2. temperaturewith heating
3. custom1.5 hours later, the reaction liquid
4. temperatureto cool
5. extractionfollowed by extraction with ethyl acetate
6. washThe organic layer was washed with a saturated sodium chloride aqueous solution
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customthe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 1/2)