HRID1882349

反应详情

EQUATION

反应方程式

HRID 1882349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.4 g of 4-(naphthalene-1-yl)phenyl boronic acid prepared by a well known method and 7.0 g of conventional 1-bromopyrene were dissolved in 80 ml of dimethoxyethane (DME). Subsequently, 0.58 g of tetrakistriphenylphosphine palladium and 40 ml of 2M-sodium carbonate aqueous solution were added therein, followed by argon displacement. After heating and refluxing over 8 hours, it was stood to cool and then an organic layer was extracted therefrom by toluene. The organic layer was washed by saturated salt water, followed by drying through anhydrous sodium sulfate, and then the organic solvent was removed by an evaporator. The residue was refined through a silica gel chromatography (a developing solvent: toluene) and then 10.0 g of 1-(4-naphthalene-1-yl-phenyl)pyrene was obtained. (yield: 99%)

WORKUP

后处理

  1. temperatureAfter heating
  2. temperaturerefluxing over 8 hours
  3. temperatureto cool
  4. extractionan organic layer was extracted
  5. washThe organic layer was washed by saturated salt water
  6. dry with materialby drying through anhydrous sodium sulfate
  7. customthe organic solvent was removed by an evaporator