HRID25746

反应详情

EQUATION

反应方程式

HRID 25746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 20.8 g of 4-bromonitrobenzene and 17.2 g of 2-methoxyphenyl boronic acid in 340 mL of ethylene glycol dimethyl ether and 170 mL of 2 M sodium carbonate solution was purged with argon gas and then 3.6 g of Pd(PPh3)2Cl2 was added under argon atmosphere. The reaction mixture was heated in a sealed flask at 120° C. overnight. The reaction mixture was cooled down to room temperature. The mixture was filtered through diatomaceous earth and the filtrate was diluted with water and the product was extracted three times with EtOAc. The organic layers were combined, dried over magnesium sulfate (MgSO4), and the solvent was evaporated in vacuo. The residue was purified by flash chromatography to yield 17.1 g of 2-methoxy-4′-nitrobiphenyl as a solid.

WORKUP

后处理

  1. customwas purged with argon gas
  2. addition3.6 g of Pd(PPh3)2Cl2 was added under argon atmosphere
  3. temperatureThe reaction mixture was cooled down to room temperature
  4. filtrationThe mixture was filtered through diatomaceous earth
  5. additionthe filtrate was diluted with water
  6. extractionthe product was extracted three times with EtOAc
  7. dry with materialdried over magnesium sulfate (MgSO4)
  8. customthe solvent was evaporated in vacuo
  9. customThe residue was purified by flash chromatography