Palladium Chloride → Bis(dibenzylideneacetone)palladium

Participants

Reaction Conditions

Reaction Steps

1.05 g palladium chloride were added to a 100 mL methanol solution containing 3.9 g sodium acetate and 4.6 g dibenzylideneacetone. The reaction mixture was warmed to 55° C. and the temperature maintained for one hour so that a precipitate was formed. The precipitate was then filtered from the methanol and redissolved in chloroform to produce a dark purple solution. This solution was stripped under reduced pressure at 25°-30° C. to produce a dark purple or black solid of Pd2DBA3.CHCl3. 1.5 g of the solid was dissolved in 100 mL THF, and added to a solution of 140-150 g of 30-5 NBR in 1.1-1.2 L THF. After 22 hours at 75°-90° C. and 350 psi hydrogen, a sample was withdrawn and a cast film IR analysis indicated that 63 percent of the olefinic NBR unsaturation had been hydrogenated.

Provenance & Evidence