HRID2186236
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 1-[(4-methoxy)phenyl]-3-(ethoxycarbonyl)-5-(methoxycarbonyl)pyrazole (4.0 g, 13.2 mmol) in 40 mL of tetrahydrofuran and 20 mL of water was added an aqueous solution of lithium hydroxide monohydrate (0.55 g, 13.2 mmol). The reaction was allowed to stir at ambient temperature for 1 h. The tetrahydrofuran was removed in vacuo and the aqueous was extracted with ether to remove unreacted diester. The aqueous layer was acidified with HCl and extracted with ethyl acetate. The organics were washed with brine, dried (MgSO4) and concentrated to afford 3.2 g (84%) of the title compound, which was used without further purification. LRMS (ES−): 289.0 (M−H)−.
WORKUP
后处理
- customThe tetrahydrofuran was removed in vacuo
- extractionthe aqueous was extracted with ether
- customto remove unreacted diester
- extractionextracted with ethyl acetate
- washThe organics were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated