Pd(dppf)Cl2的制备

发布时间： 2019-05-13

Toabsolute acetonitrile (1950 mL) degassed via three vacuum/nitrogen ingresscycle was added dichloropalladium (13 g,73 mmol), the mixture was refluxed at 90~100 °C overnight. The reactant was concentrated toobtain Pd(CH₃CN)₂Cl₂ as orange solid.  To a suspension of Pd(CH₃CN)₂Cl₂(19 g, 73 mmol) in benzene (680mL) was added a solution of dppf (40.6 g,73 mmol) in benzene (680 mL), the mixture was stirred at rt overnight, thereddish brown precipitate formed was collected by filtration, washed withbenzene, and dried in vacuo to give Pd(dppf)₂Cl₂ (~48 g) in over 90% yield.  This is pure enough for the next step, thecomplex can be recrystallized from chloroform/benzene.