HRID83494
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1-(4-fluorophenyl)-5-(3-(trifluoromethoxy)phenyl)-4,5-dihydro-1H-pyrazol-3-ylamine (1.29 g) in toluene (10 ml) was added activated carbon (pH5 to 8, 0.64 g), and the mixture was stirred for 2 hours under oxygen atmosphere under cooling to reflux. After cooling to room temperature, the activated carbon was filtered off through Celite eluting with ethyl acetate. This filtrate was concentrated under reduced pressure. To the resulting residue, a mixed solvent of diisopropyl ether/n-hexane was added and the mixture was stirred at room temperature. The insoluble substance was collected by filtration, and then dried under reduced pressure to give the titled compound (652 mg).
WORKUP
后处理
- temperatureunder cooling
- temperatureto reflux
- filtrationthe activated carbon was filtered off through Celite
- washeluting with ethyl acetate
- concentrationThis filtrate was concentrated under reduced pressure
- additionTo the resulting residue, a mixed solvent of diisopropyl ether/n-hexane was added
- stirringthe mixture was stirred at room temperature
- filtrationThe insoluble substance was collected by filtration
- customdried under reduced pressure