反应详情

温度

120 °C

Ethyl 1-(4-fluorophenyl)-5-hydroxypyrazole-4-carboxylate (1 g) and 5-amino-2-isobutoxybenzonitrile (0.8 g) were added to pyridine (10 ml) and the mixture was stirred at 120° C. for 4 h. After evaporation of the solvent under reduced pressure, hydrochloric acid was added to the residue and the mixture was extracted with chloroform. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the residue to allow crystallization. The crystals were recrystallized from a mixed solvent of ethanol-diisopropyl ether to give the title compound (0.2 g), melting point: 207–208° C.

1. customAfter evaporation of the solvent under reduced pressure, hydrochloric acid
2. additionwas added to the residue
3. extractionthe mixture was extracted with chloroform
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customafter which the solvent was evaporated under reduced pressure
7. additionDiisopropyl ether was added to the residue
8. customcrystallization
9. customThe crystals were recrystallized from a mixed solvent of ethanol-diisopropyl ether