HRID12819
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 (20 g, 91.2 mmol; available from Butt Park Ltd., Camelford, Cornwall, UK) in methanol (100 mL) and water (100 mL) was added LiOH (2.4 g, 100 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