HRID1530740

反应详情

EQUATION

反应方程式

HRID 1530740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

90 g (244 mmol) 9-Phenyl-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-9H-carbazole and 69 g (244 mmol) 1-Iodo-4-Brombenzene [589-87-7] are dissolved in 500 ml toluene treated with 200 ml of a 2 M solution of sodium carbonate. The reaction mixture is carefully degassed and 200 mg tetrakistriphenylphosphine palladiume are added. The reaction is heated to reflux for 20 h. The solution is then cooled to room temperature and the layers are separated. The water phase is extracted three times with toluene, and then the organic layers is washed twice with water dried over magnesium sulphate, filtrated and the solvent is removed in the vacuum. The residue is recrystallized from DMF, to yield 100 g (225 mmol) (92%) of a with powder with a purity of 98.7%.

WORKUP

后处理

  1. customThe reaction mixture is carefully degassed
  2. addition200 mg tetrakistriphenylphosphine palladiume are added
  3. temperatureThe reaction is heated
  4. temperatureto reflux for 20 h
  5. customthe layers are separated
  6. extractionThe water phase is extracted three times with toluene
  7. washthe organic layers is washed twice with water
  8. dry with materialdried over magnesium sulphate
  9. filtrationfiltrated
  10. customthe solvent is removed in the vacuum
  11. customThe residue is recrystallized from DMF
  12. customto yield 100 g (225 mmol) (92%) of a with powder with a purity of 98.7%