反应详情

温度

0 °C

A suspension of 4,5-diamino-1-methylpyrazole sulfuric acid salt (20 g) in triethylamine (29.2 ml) was stirred at 0° C. for 10 minutes. A mixture of acetic anhydride (9.87 ml) and formic acid (7.96 ml) was stirred at 40° C. for 30 minutes, cooled to 0° C., and added dropwise to the above solution at 0° C. The whole mixture was stirred at 0° C. for 2 hours. To the mixture was added brine, and the whole mixture was extracted with tetrahydrofuran. The organic layer was dried over magnesium sulfate and evaporated under reduced pressure to give crude N-(5-amino-1-methyl-1H-pyrazol-4-yl)formamide, which was used in the next step without further purification.

1. stirringwas stirred at 40° C. for 30 minutes
2. temperaturecooled to 0° C.
3. additionadded dropwise to the above solution at 0° C
4. stirringThe whole mixture was stirred at 0° C. for 2 hours
5. extractionthe whole mixture was extracted with tetrahydrofuran
6. dry with materialThe organic layer was dried over magnesium sulfate
7. customevaporated under reduced pressure