HRID1615885

反应详情

EQUATION

反应方程式

HRID 1615885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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)propoxy]-5-methylpyrazole-3-carboxylic acid ethyl ester.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. additionEtOAc was added to the residue
  3. washthe organic layer was washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. customAfter the evaporation of the solvent
  6. customthe obtained residue was purified by silica gel column chromatography (eluent: hexane-EtOAc=15:1˜5:1)