HRID83494

反应详情

EQUATION

反应方程式

HRID 83494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder cooling
  2. temperatureto reflux
  3. filtrationthe activated carbon was filtered off through Celite
  4. washeluting with ethyl acetate
  5. concentrationThis filtrate was concentrated under reduced pressure
  6. additionTo the resulting residue, a mixed solvent of diisopropyl ether/n-hexane was added
  7. stirringthe mixture was stirred at room temperature
  8. filtrationThe insoluble substance was collected by filtration
  9. customdried under reduced pressure