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

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

7synthesis methods

Product Name:Bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II)
CAS Number:887919-35-9
Molecular formula:C32H58Cl2N2P2Pd
Molecular Weight:710.1

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.

14592-56-4
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$22.00/100mg

932710-63-9 Synthesis

Bis(di-tert-butyl)-4-dimethylaminophenylphosphine

932710-63-9
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$11.00/250mg

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

887919-35-9
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$20.00/250mg

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

12107-56-1 Synthesis