反应 #41104

反应方程式

t-butylhydrazine hydrochloride salt

ethyl (ethoxymethylene)-cyanoacetate

sodium acetate

→

5-amino-1-tert-butyl-1H-pyrazole-4-carboxylic acid ethyl ester

收率 77.0%

溶剂

ethanol

反应条件

后处理

1. 1
   温度refluxed for 16 hours
2. 2
   萃取The separated aqueous phase was extracted three times with dichloromethane
3. 3
   洗涤The combined organic phases were washed successively with water and saturated brine solution
4. 4
   干燥dried with sodium sulfate
5. 5
   其他The solvent was removed in vacuo

实验过程

A solution containing t-butylhydrazine hydrochloride salt (10 g, 80.3 mmol), ethyl (ethoxymethylene)-cyanoacetate (13.6 g, 80.4 mmol), and anhydrous sodium acetate (8.2 g, 100 mmol) in 100 mL ethanol was stirred and refluxed for 16 hours. The solution was poured into ice-water. The separated aqueous phase was extracted three times with dichloromethane. The combined organic phases were washed successively with water and saturated brine solution and dried with sodium sulfate. The solvent was removed in vacuo to give 5-amino-1-tert-butyl-1H-pyrazole-4-carboxylic acid ethyl ester (13 g, 77%).

来源