HRID1013055
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 2-(4-Methoxy-phenyl)-5-methyl-2H-pyrazole-3-carboxylic acid ethyl ester (400 mg) in a 1:1:1 mixture of MeOH:THF:water was added 10% NaOH (20 mL). The mixture was heated to reflux and the reaction monitored by TLC and HPLC until hydrolysis was complete. The solution was cooled and concentrated under reduced pressure. The residue was acidified with 10% HCl and extracted with EtOAc. The organic fractions were combined and dried over MgSO4 and concentrated under reduced pressure. The resulting solid was used without further purification (Yield 242 mg). LC-MS (C12H12N2O3 calculated 232) m/z 231 (M−H).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux
- customthe reaction monitored by TLC and HPLC until hydrolysis
- temperatureThe solution was cooled
- concentrationconcentrated under reduced pressure
- extractionextracted with EtOAc
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
- customThe resulting solid was used without further purification (Yield 242 mg)