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Pd(dppf)Cl2的制备

Pd(dppf)Cl2的制备

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.