HRID1639935

反应详情

EQUATION

反应方程式

HRID 1639935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Under a nitrogen stream, 5.0 g (0.032 mol) of 4-chloro-phenyl boronic acid, 10.0 g (0.064 mol) of 2-bromopyridine, 150□ of tetrahydrofuran and 2M potassium carbonate solution (20□) were placed into a 2-neck round flask 250□ and then 0.37 g (3 mol %) of palladium tetrakistriphenylphosphine [(pd(PPh3)4] was added as a catalyst. After the resulting solution was heated to reflux at 80° C. for 24 hours, the reaction was terminated. The resulting mixture was poured into a beaker containing 200□ of distilled water. After extraction with ether (150□) three times, 10 g of magnesium sulfate was added. The resulting solution was stirred by a rotary stirrer for 30 minutes and then the extraction mixture was filtered. After removing the solvent using a rotary evaporator, the residue was subjected to column chromatography using dichloromethane as a developing solvent and then distilled under reduced pressure to give the 2-(4-chloro-phenyl)pyridine. The yield was 56%.

WORKUP

后处理

  1. temperatureAfter the resulting solution was heated
  2. customthe reaction was terminated
  3. additionThe resulting mixture was poured into a beaker
  4. additioncontaining 200□ of distilled water
  5. extractionAfter extraction with ether (150□) three times, 10 g of magnesium sulfate
  6. additionwas added
  7. filtrationthe extraction mixture was filtered
  8. customAfter removing the solvent
  9. customa rotary evaporator
  10. distillationdistilled under reduced pressure