HRID1269633

反应详情

EQUATION

反应方程式

HRID 1269633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of 2,6-dichloropyrazine (3 g, 20 mmol), sodium carbonate (5.55 g, 52 mmol) and 4-methylphenylboronic acid (2.74 g 20 mmol) in dimethoxyethane (90 mL) and water (45 mL) under nitrogen was added tetrakis(triphenylphosphine) palladium (0) (0.46 g). The resulting mixture was heated at reflux for 18 h under nitrogen. After cooling to room temperature, the reaction was diluted with water (100 mL) and extracted with chloroform (2×150 mL). The organic solution was dried MgSO4 and the solvents removed in vacuo. Purification by Biotage™ chromatography (Silica, 90 g) 9:1 cyclohexane:EtOAc afforded the title compound as a white solid (2.3 g).

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 18 h under nitrogen
  3. extractionextracted with chloroform (2×150 mL)
  4. customthe solvents removed in vacuo
  5. customPurification by Biotage™ chromatography (Silica, 90 g) 9:1 cyclohexane