HRID1773059

反应详情

EQUATION

反应方程式

HRID 1773059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In a stream of argon, 1.13 g of 2-chloro-1,10-phenanthroline, 1.57 g of 2,4-di(3-biphenylyl-6-[3,5-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-phenyl]-1,3,5-triazine, 280 mg of lithium chloride and 203 mg of tetrakis(triphenylphosphine)palladium were suspended in a toluene (60 mL)/ethanol (15 mL) mixed solvent. 8.8 mL of a 2.0 M aqueous sodium carbonate solution was added in the obtained suspension, and the mixture was stirred at 100° C. for 65 hours. Then the reaction mixture was left to be cooled to room temperature, and distilled under a reduced pressure to remove low-boiling point ingredients. The thus-obtained residue was purified by alumina column chromatography using chloroform as a developing solvent to give 1.22 g of target 2,4-di(3-biphenylyl-6-[3,5-bis(1,10-phenanthrolin-2-yl)phenyl]-1,3,5-triazine as a white powder (yield, 68%).

WORKUP

后处理

  1. additionmixed solvent
  2. waitThen the reaction mixture was left
  3. temperatureto be cooled to room temperature
  4. distillationdistilled under a reduced pressure
  5. customto remove low-boiling point ingredients
  6. customThe thus-obtained residue was purified by alumina column chromatography
  7. customto give 1.22 g of target 2,4-di(