HRID1160050

反应详情

EQUATION

反应方程式

HRID 1160050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 500-ml four-necked flask were placed 22.4 g (0.10 mole) of 1,3-diphenylpropanedione, 20.0 g (0.13 mole) of p-nitrophenylhydrazine, and 200.7 g of toluene. The mixture was then heated under reflux with stirring for three hours. Upon completion of the reaction, the reaction mixture was cooled to room temperature and a solid was recovered by filtration. The filtrate was concentrated under reduced pressure to dryness. The residue was purified by reslurrying by adding 300 ml of methanol. Thereafter, the residue was cooled to room temperature and a solid was recovered by filtration. The solid was washed with methanol and dried under reduced pressure to give 26.0 g of 1-(p-nitrophenyl)-3,5-diphenylpyrazole.

WORKUP

后处理

  1. customIn a 500-ml four-necked flask were placed
  2. temperatureThe mixture was then heated
  3. temperatureunder reflux
  4. customUpon completion of the reaction
  5. filtrationa solid was recovered by filtration
  6. concentrationThe filtrate was concentrated under reduced pressure to dryness
  7. customThe residue was purified
  8. additionby adding 300 ml of methanol
  9. temperatureThereafter, the residue was cooled to room temperature
  10. filtrationa solid was recovered by filtration
  11. washThe solid was washed with methanol
  12. customdried under reduced pressure