HRID1514007

反应详情

EQUATION

反应方程式

HRID 1514007 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In an atmosphere of argon, 496 g (2.46 mol) of 5-bromosalicylaldehyde, 361 g (2.96 mol) of phenylboronic acid, 57 g (49.0 mmol) of tetraxis(triphenylphosphine)palladium(0), 8.6 L of DME and 784 g of sodium carbonate/3.7 L of water were charged, and subjected to heating under reflux with stirring for 17 hours. After cooling the resultant to room temperature, 3 L of toluene was added, and then an aqueous layer was removed. An organic layer was washed with water, and dried with magnesium sulfate. The solvent was distilled off under a reduced pressure. The crystals were purified by silica gel chromatography, whereby 382 g of 3-formyl-4-hydroxybiphenyl was obtained (yield: 78%).

WORKUP

后处理

  1. temperatureto heating
  2. temperatureunder reflux
  3. customan aqueous layer was removed
  4. washAn organic layer was washed with water
  5. dry with materialdried with magnesium sulfate
  6. distillationThe solvent was distilled off under a reduced pressure
  7. customThe crystals were purified by silica gel chromatography