HRID2091440

反应详情

EQUATION

反应方程式

HRID 2091440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

4-(diphenylamino)phenylboronic acid (4.87 g, 16.8 mmol), 4-bromo-N-phenylaniline (3.5 g, 14 mmol), potassium phosphate (9.2 g, 42 mmol), dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (0.23 g, 0.56 mmol) were added to a three-neck flask under nitrogen. 200 mL of toluene and 20 mL of water was then added. The solution was degassed with nitrogen for 20 minutes. Pd2(dba)3 (0.13 g, 0.14 mmol) was added to the mixture. The mixture was then heated up to reflux overnight. After cooled to room temperature, the organic layer was separated and dried over magnesium sulfate. After evaporating solvent, the residue was purified by column chromatography using 1:2 dichloromethane and hexanes as eluent. 4.7 g of desired product was obtained. (81% yield)

WORKUP

后处理

  1. customThe solution was degassed with nitrogen for 20 minutes
  2. temperatureThe mixture was then heated up
  3. temperatureto reflux overnight
  4. customthe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. customAfter evaporating solvent
  7. customthe residue was purified by column chromatography