HRID2067950
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of ethyl acetoacetate (8.0 mL, 63 mmol) and dimethylformamide-dimethylacetal (8.3 mL, 63 mmol) is heated to reflux for 1 hour. The reaction mixture is cooled to room temperature and diluted with EtOH (70 mL). Hydrazine hydrate (3.0 mL, 63 mmol) is then added and the reaction is heated at 80° C. for 2 hours. The resultant solution is cooled to room temperature and concentrated in vacuo to afford crude 5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester which is used without further purification.
WORKUP
后处理
- temperatureis heated
- temperatureto reflux for 1 hour
- temperaturethe reaction is heated at 80° C. for 2 hours
- concentrationconcentrated in vacuo