HRID349527
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 ethyl 3-(1-methyl-5-triphenylmethylaminopyrazol-4-yl)propionate (22 g, 50 mmol) in methanol (60 ml) was added 10% aqueous sodium hydroxide solution (60 ml), and the mixture was stirred under reflux for 2 hours. The reaction mixture was acidified with 10% aqueous citric acid solution, and the mixture was extracted with a mixed solvent of chloroform and methanol. The extract was dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue was triturated with diisopropyl ether and dried in vacuo to give 3-(1-methyl-5-triphenylmethylaminopyrazol-4-yl)propionic acid (16 g) as a colorless solid.
WORKUP
后处理
- temperatureunder reflux for 2 hours
- extractionthe mixture was extracted with a mixed solvent of chloroform and methanol
- dry with materialThe extract was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was triturated with diisopropyl ether
- customdried in vacuo