反应详情

0.13 g of 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxamide was added to a 1,4-dioxane 6 ml solution comprising 0.14 g of 2,3-dichloro-5,6-dicyano-p-benzoquinone, followed by reflux with heating for 18 hours. After the reaction liquid was stood to cool, it was poured to water, followed by extraction with ethyl acetate, and the organic layer was washed with a saturated sodium chloride aqueous solution and dried over sodium sulfate. The filtrate was distilled under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=8/2 to 7/3) to obtain 33 mg of the desired product (melting point: 231 to 233° C.).

1. temperatureby reflux
2. temperaturewith heating for 18 hours
3. customAfter 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 sodium sulfate
8. distillationThe filtrate was distilled under reduced pressure
9. customthe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=8/2 to 7/3)