تفاعل #41104

معادلة التفاعل

t-butylhydrazine hydrochloride salt

ethyl (ethoxymethylene)-cyanoacetate

sodium acetate

→

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

المردود 77.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed for 16 hours
2. 2
   استخلاصThe separated aqueous phase was extracted three times with dichloromethane
3. 3
   غسيلThe combined organic phases were washed successively with water and saturated brine solution
4. 4
   تجفيفdried with sodium sulfate
5. 5
   أخرىThe solvent was removed in vacuo

الإجراء التجريبي

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%).

المصدر