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ChemicalBook CAS DataBase List Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II)
887919-35-9

Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) synthesis

7synthesis methods
To a 500 mL reaction was added 10 g (1,5-cyclooctadiene) palladium dichloride, the reaction flask was replaced with a nitrogen atmosphere,19.6 g of di-tert-butyl-4-dimethylaminophenylphosphine and 200 mL of anhydrous tetrahydrofuran were added. The mixture was stirred at room temperature for 16 hours; There was a solid precipitation; filtration and drying gave a pale yellow powder product bis (di-tert-butyl-4-dimethylaminophenylphosphine) palladium chloride. The yield was 97 percent.
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Yield:887919-35-9 1445 g

Reaction Conditions:

in tetrahydrofuran at 20; for 9.5 h;Inert atmosphere;

Steps:

1

Take a dry 10L three-neck reaction flask, dry nitrogen is fully replaced and under nitrogen flow protection,Add 5.5 L of anhydrous tetrahydrofuran, stir and add 540 g of bis(acetonitrile)palladium dichloride.The obtained ligand di-tert-butyl-4-dimethylaminophenylphosphine was further reacted for 30 minutes, and a yellow solid was precipitated. After the reaction was continued for 9 hours at room temperature,After filtration, the filter cake was dipped in anhydrous tetrahydrofuran, drained and dried in a vacuum oven at 60 ° C.Obtaining a yellow crystalline powdery target product, namely dichlorodi-tert-butyl-(4-dimethylaminophenyl)phosphine palladium, yielding 1440 g to 1445 g,Elemental analysis showed that the product content exceeded 98.0%, the palladium content exceeded 15.0%, and the palladium calculated yield was 97.7% to 98.1%.

References:

CN108659054,2018,A Location in patent:Paragraph 0057; 0061

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