反应详情

5-Methylisoxazole-4-carbonyl chloride (1.4 g) synthesized according to the method described in J. Chem. Soc. Perkin Trans. I, pp. 1875–1879 (1988) was added to a pyridine solution (20 ml) containing N-[3-cyano-4-(piperazin-1-yl)phenyl]-1-(4-fluorophenyl)-5-methylpyrazole-4-carboxamide (4 g) under ice-cooling, and the mixture was stirred for 1 h. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with dilute hydrochloric acid and saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under pressure. Diisopropyl ether was added to the obtained residue to allow crystallization. The crystals were recrystallized from hydrous dimethylformamide to give the title compound (2.9 g), melting point: 208° C.

1. temperaturecooling
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with dilute hydrochloric acid and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customafter which the solvent was evaporated under pressure
6. additionDiisopropyl ether was added to the obtained residue
7. customcrystallization
8. customThe crystals were recrystallized from hydrous dimethylformamide