Synthesis of palladium dibenzylideneacetone; Bis(dibenzylideneacetone)palladium
Submitted Aug 15, 2001, published Aug 15, 2001
Palladium dichloride (strem),
Sodium acetate trihydrate (Aldrich, 99+%),
Dibenzylideneacetone (4.60 g, 19.6 mmol) and sodium acetate trihydrate (6.47 g, 47.5 mmol) were placed in a one necked 500 mL round bottomed flask with a sidearm and the flask fitted with a stopper. The side arm was attached to a double manifold Schlenk line and the flask cycled three times vacuum/Argon. Under a flow of argon the stopper was removed, methanol (150 mL) was added and the flask re-stoppered. The reactants were dissolved at 50 oC. Under a flow of argon the stopper was removed for a second time, PdCl2 (1.05 g, 5.9 mmol) was added and the flask was re-stoppered again. The side arm tap and Schlenk line tap were both left open to argon. An oil bubbler was attached to a second tap of the Schlenk line and the tap opened to argon. The mixture was heated at 40 oC with stirring under an oil bubbler presure of argon for 4 h after which a dark purple/black precipitate had formed. The precipitate was collected by filtration on a Buchner funnel and washed 1st with water (70 mL) and 2nd with acetone (70 mL). The product was dried under vacuum to yield 3.12 g of a dark purple solid (92% yield).
No data has been collected on this product as common analytical methods do not help in establishing the stoichiometry of the product. The Previously published work has shown the various stoichiometries to be correct by means of X-ray diffraction studies and elemental analysis (see refs.).
Toshinao, U.; Kawazura, H.; Ishii, Y. J. Organomet. Chem., 1974, 65, 253.
Takahashi, Y.; Ito, T.; Sakai, S.; Ishii, Y. J. Chem. Soc. Chem. Commun., 1970, 1065.
Keywords: dba, dibenzylideneacetone, palladium