تفاعل #1747913

معادلة التفاعل

ethyl acetoacetate

acetic acid

5-methyl-2H-pyrazol-3-ylamine

→

solid

المردود 101.9%

2,5-Dimethyl-4H-pyrazolo[1,5-a]pyrimidin-7-one

المردود 101.9%

المذيبات

tert-butyl methyl ether

ظروف التفاعل

المعالجة

1. 1
   أخرىat 25-28° C
2. 2
   درجة الحرارةHeat the mixture
3. 3
   درجة الحرارةat reflux for 10 h
4. 4
   workup.ADDITIONAdd
5. 5
   درجة الحرارةcooled to 5° C.
6. 6
   أخرىthe temperature below 10° C
7. 7
   ترشيحfilter
8. 8
   أخرىDry the resulting material in vacuo overnight

الإجراء التجريبي

Add ethyl acetoacetate (128 g, 0.98 mol) dropwise to an acetic acid solution (500 mL) of 5-methyl-2H-pyrazol-3-ylamine (100 g, 0.95 mol), keeping the temperature at 25-28° C. Heat the mixture at reflux for 10 h and then cool to room temperature. Add the reaction to tert-butyl methyl ether (5 L) cooled to 5° C., keeping the temperature below 10° C. Stir for 1 h at 5° C., and filter. Dry the resulting material in vacuo overnight to provide a white solid (158 g, 96%).

المصدر