HRID405237

反应详情

EQUATION

反应方程式

HRID 405237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Ethyl 3-(5-bromopicolinamido)propanoate (2.2 g, 7.3 mmol), (5-chloro-2-formylphenyl)boronic acid (1.4 g, 7.7 mmol), Pd(dppf)Cl2 (810 mg, 1.1 mmol), and K2CO3 (2.3 g, 16.9 mmol) and PdCl2(dppf) were dissolved in wet DMF (10 mL) and the resulting mixture was heated to 90° C. After 16 h the resulting mixture was cooled to room temperature, filtered through CELITE and the filtrate was diluted with EtOAc, washed with water and sat. aqueous NaHCO3. The organic layer was dried (Na2SO4), concentrated and purified via column chromatography to yield the title compound.

WORKUP

后处理

  1. temperatureAfter 16 h the resulting mixture was cooled to room temperature
  2. filtrationfiltered through CELITE
  3. additionthe filtrate was diluted with EtOAc
  4. washwashed with water and sat. aqueous NaHCO3
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. concentrationconcentrated
  7. custompurified via column chromatography