HRID1804130

反应详情

EQUATION

反应方程式

HRID 1804130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a mixture of 4-(5-bromopyridin-2-yl)piperazine-1-carboxylic acid tert-butyl ester (5.37 g), bis(tricyclohexylphosphine)palladium (II) dichloride (347 mg), tripotassium phosphate (9.99 g) and cyclopropylboronic acid (2.02 g) were added toluene (49 mL) and water (2.5 mL), and the mixture was refluxed. After cooling, ethyl acetate and saturated aqueous sodium hydrogen carbonate solution were added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate, and the solvent was evaporated. The residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (3.41 g).

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureAfter cooling
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over sodium sulfate
  6. customthe solvent was evaporated
  7. customThe residue was purified by column chromatography (hexane:ethyl acetate)