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
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
- customIn a 500-ml four-necked flask were placed
- temperatureThe mixture was then heated
- temperatureunder reflux
- customUpon completion of the reaction
- filtrationa solid was recovered by filtration
- concentrationThe filtrate was concentrated under reduced pressure to dryness
- customThe residue was purified
- additionby adding 300 ml of methanol
- temperatureThereafter, the residue was cooled to room temperature
- filtrationa solid was recovered by filtration
- washThe solid was washed with methanol
- customdried under reduced pressure