HRID1840694

反应详情

EQUATION

反应方程式

HRID 1840694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Thereafter, to 200 ml of diisopropylamine were added 15.54 g (0.032 mol of tri(4-bromophenyl)amine, 1.35 g (1.92 mmol) of bis[triphenylphosphin]palladium dichloride and 9.43 g (0.96 mmol) of copper iodide. After the reaction mixture was stirred for 2 h at room temperature, 9.43 g, (96 mmol) of trimethylsilyl acetylene was slowly added to the reaction mixture. The reaction mixture was refluxed for 8 h and cooled. Solvent was removed under the reduced pressure. The residue was extracted with benzene and the benzene layer was washed with distilled water. The washed benzene layer was concentrated to give 13.84 g (81%) of tri(4-trimethylsilylethynylphenyl)amine.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 8 h
  2. temperaturecooled
  3. customSolvent was removed under the reduced pressure
  4. extractionThe residue was extracted with benzene
  5. washthe benzene layer was washed with distilled water
  6. concentrationThe washed benzene layer was concentrated