HRID1869575
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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of 1.96 g of 5-methylpyrazole-3-carboxylic acid ethyl ester in 40 ml of DMF, 2.64 g of potassium carbonate and 3.53 ml of 3-(tert-butyldimethylsilyloxy)propylbromide were added, and the mixture was stirred at 50° C. for 18 hours. The solvent was evaporated, EtOAc was added to the residue, and the organic layer was washed with water and brine and dried over sodium sulfate. After the evaporation of the solvent, the obtained residue was purified by silica gel column chromatography (eluent: hexane-EtOAc=15:1˜5:1) to obtain 1.39 g of 1-[3-(tert-butyldimethylsilyloxy)propoxyl]-5-methylpyrazole-3-carboxylic acid ethyl ester.
WORKUP
后处理
- customThe solvent was evaporated
- additionEtOAc was added to the residue
- washthe organic layer was washed with water and brine
- dry with materialdried over sodium sulfate
- customAfter the evaporation of the solvent
- customthe obtained residue was purified by silica gel column chromatography (eluent: hexane-EtOAc=15:1˜5:1)