HRID322851
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 solution of ethyl 2-benzyl-5-(4-benzyloxyphenyl)-2H-pyrazole-3-carboxylate (1.2 g) in methanol (125 mL) is treated with 10% aqueous potassium hydroxide solution (10 mL, w/v) and the mixture is heated to reflux for 2 hours. The reaction mixture is evaporated in vacuo, stirred with 1N hydrochloric acid (50 mL) and extracted with ethyl acetate (100 mL). The organic phase is dried over magnesium sulphate, evaporated in vacuo, and the residue crystallised from a mixture of ethyl acetate and cyclohexane to give 2-benzyl-5-(4-benzyloxyphenyl)-2H-pyrazole-3-carboxylic acid (0.55 g), m.p. 207-208° C. [Elemental analysis:- C,75.2; H,5.20; N,7.30%. Calculated:- C,75.0; H,5.20; N,7.30%].
WORKUP
后处理
- temperaturethe mixture is heated
- temperatureto reflux for 2 hours
- customThe reaction mixture is evaporated in vacuo
- extractionextracted with ethyl acetate (100 mL)
- dry with materialThe organic phase is dried over magnesium sulphate
- customevaporated in vacuo
- customthe residue crystallised from a mixture of ethyl acetate and cyclohexane