反应详情

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%).

1. customat 25-28° C
2. temperatureHeat the mixture
3. temperatureat reflux for 10 h
4. additionAdd
5. temperaturecooled to 5° C.
6. customthe temperature below 10° C
7. filtrationfilter
8. customDry the resulting material in vacuo overnight