反应详情

温度

70 °C

1.0 g of N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-5-oxopyrazolidine-3-carboxamide was dissolved in 10 mL of N,N-dimethylformamide, and 460 mg of 2,3-dichloropyridine and then 350 mg of sodium hydride were added, followed by stirring at about 70° C. for about 7 hours in a nitrogen atmosphere, and then the reaction liquid was left to cool. To the reaction liquid, water and ethyl acetate were added, followed by stirring and extraction with ethyl acetate. Then, concentration under reduced pressure was carried out to obtain a crude product. The crude product was purified by silica gel column chromatography (eluent: ethyl acetate/ethanol=9/1) to obtain 1.15 g of the desired product (melting point: 165-167° C.).

1. customthe reaction liquid
2. waitwas left
3. temperatureto cool
4. additionwere added
5. stirringby stirring
6. extractionextraction with ethyl acetate
7. concentrationThen, concentration under reduced pressure
8. customto obtain a crude product
9. customThe crude product was purified by silica gel column chromatography (eluent: ethyl acetate/ethanol=9/1)