HRID2274123

反应详情

EQUATION

反应方程式

HRID 2274123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under the atmosphere of argon, 230 g of 1,4-dibromonaphthalene, 121 g of 2-formylphenylboronic acid and 18.5 g of tetrakis(triphenylphosphine)palladium(0) were placed in a flask. To the resulting mixture, 2.4 L of dimethoxyethane (DME) and 1.2 L of an aqueous 2M sodium carbonate solution were added, followed by stirring under reflux for 8 hours. After cooling to the room temperature, an aqueous phase was removed, and an organic phase was washed with water and saturated saline, and dried with magnesium sulfate. After filtering off magnesium sulfate, the organic phase was concentrated. The residues were purified by silica gel column chromatography, whereby 170 g (yield 67%) of 1-bromo-4-(2-formylphenyl)naphthalene as an intended product was obtained.

WORKUP

后处理

  1. temperatureunder reflux for 8 hours
  2. customan aqueous phase was removed
  3. washan organic phase was washed with water and saturated saline
  4. dry with materialdried with magnesium sulfate
  5. filtrationAfter filtering off magnesium sulfate
  6. concentrationthe organic phase was concentrated