반응 #41104

반응 방정식

t-butylhydrazine hydrochloride salt

ethyl (ethoxymethylene)-cyanoacetate

sodium acetate

→

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

수율 77.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도refluxed for 16 hours
2. 2
   추출The separated aqueous phase was extracted three times with dichloromethane
3. 3
   세척The combined organic phases were washed successively with water and saturated brine solution
4. 4
   건조dried with sodium sulfate
5. 5
   기타The solvent was removed in vacuo

실험 절차

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%).

출처