反应 #1076769

反应方程式

diethyl malonate

1,2-diphenylhydrazine

methanol

sodium methoxide

→

1,2-diphenyl-3,5-pyrazolidinedione

收率 68.7%

溶剂

n-butanol

反应条件

后处理

1. 1
   workup.DISTILLATIONSubsequently, the solvent was distilled off under reduced pressure, 10 ml of water
2. 2
   workup.ADDITIONwas added
3. 3
   过滤the reaction solution was filtered
4. 4
   workup.ADDITIONAn activated carbon was added to the recovered filtrate
5. 5
   workup.STIRRINGstirred for 30 minutes
6. 6
   workup.STIRRINGAfter stirring
7. 7
   过滤the solution was filtered again
8. 8
   其他to recover the filtrate
9. 9
   workup.ADDITIONFour (4) ml of hydrochloric acid was added to the filtrate
10. 10
    过滤the precipitated solid was recovered by filtration

实验过程

Three point six five (3.65) grams (22.8 mmol) of diethyl malonate and 4.00 g (21.7 mmol) of 1,2-diphenylhydrazine were dissolved in 10 ml of n-butanol, then 4.61 g (23.9 mmol) of a 28% methanol solution of sodium methoxide was added thereto, and the reaction system was heated at 100° C. for 10 hours. Subsequently, the solvent was distilled off under reduced pressure, 10 ml of water was added thereto and stirred, and then the reaction solution was filtered. An activated carbon was added to the recovered filtrate and stirred for 30 minutes. After stirring, the solution was filtered again to recover the filtrate. Four (4) ml of hydrochloric acid was added to the filtrate, and the precipitated solid was recovered by filtration. Thus, 3.76 g (yield: 60%) of 1,2-diphenyl-3,5-pyrazolidinedione was obtained.

来源