HRID385309

反应详情

EQUATION

反应方程式

HRID 385309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

12.9 g (28.5 mmol) 3-(triphenylen-2-yl)phenyl trifluoromethanesulfonate, 6.5 g (42.8 mmol) 3-methoxyphenylboronic acid, 0.47 g (1.1 mmol) 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (SPhos) and 18.2 g (85.5 mmol) potassium phosphate tribasic (K3PO4) were weighed in a round bottom flask. 150 mL toluene and 80 mL water were added to the flask as solvent. The solution was purged with nitrogen and 0.26 g (0.28 mmol) of tris(dibenzylideneacetone)dipalladium (0) [Pd2(dba)3] was added. The solution was heated to reflux for twelve hours. Upon cooling, the organic layer was separated, and dried with MgSO4. The product was readily separated by column chromatography using hexane/dichloromethane as eluent (1/0 gradient to 3/2). The solvent was removed by rotary evaporation resulting in 11.7 g (28 mmol) of the product, 2-(3′-methoxybiphenyl-3-yl)triphonylene.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe solution was heated
  3. temperatureto reflux for twelve hours
  4. temperatureUpon cooling
  5. customthe organic layer was separated
  6. dry with materialdried with MgSO4
  7. customThe product was readily separated by column chromatography
  8. customThe solvent was removed by rotary evaporation