HRID1393043
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
To a solution of 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carboxylic acid ethyl ester (Maybridge plc, Cornwall, UK; 20 g, 91.2 mmol) in methanol (100 mL) and water (100 mL) was added LiOH (2.4 g, 100.3 mmol). The reaction mixture was stirred at reflux for 4 hours and then concentrated under reduced pressure to remove the methanol. The residue was diluted with water, acidified to pH 2 with concentrated HCl (9 mL), and extracted with ethyl acetate. The combined extracts were evaporated in vacuo to give 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carboxylic acid which was used without further purification.
WORKUP
后处理
- temperatureat reflux for 4 hours
- concentrationconcentrated under reduced pressure
- customto remove the methanol
- additionThe residue was diluted with water
- extractionextracted with ethyl acetate
- customThe combined extracts were evaporated in vacuo