Allyl palladium chloride dimer from an allyl chloride; Bis(Methallyl)di-chloro-dipalladium(II)
Submitted Aug 15, 2001, published Aug 15, 2001
Palladium chloride (Strem),
Methallyl chloride (Aldrich, isomeric mixture),
CO (Air products, technical grade).
A 500 ml one necked round bottomed flask with a sidearm was fitted with a stir bar and charged with PdCl2 (4.44 g, 25 mmol), NaCl (2.96 g, 50 mmol), H2O (20 mL) and MeOH (60 mL). The mixture was stirred for 10 min to allow formation of an aqueous solution. Methallyl Chloride (7.10 g, 78 mmol) was added to the solution and a septum fitted to the flask. A needle, connected to a CO cylinder, was inserted into the septum and the tip placed in the solution. CO was bubbled through the solution and vented via a bubbler attached to the sidearm. The mixture was left to stir for 1 h during which time a colour change was observed from reddish brown to yellow as a flocculent yellow solid precipitated. The yellow suspension was poured into water (300 mL) and the product extracted with chloroform (3 x 100 mL). The chloroform extract was washed with water (3 x 50 mL) and dried over MgSO4. The solvent was removed in vacuo to yield a yellow solid which was recrystallized from a chloroform/hexane layered system to yield the product as a yellow, crystalline air stable solid. 4.12 g of product were obtained (84 % yield).
1H nmr (C6D6): 1.38 (3H, s, CH3), 2.32 (2H, d) 3.41, (2H, d) (syn and anti terminal allyl H's)
Tatsuno, Y.; Yoshida, T.; Otsuka, S. Inorg. Synth., John Wiley & Sons, 1990, 28, 342.
Tatsuno, Y.; Yoshida, T.; Otsuka, S. Inorg. Synth., John Wiley & Sons, 1979, 19, 220.
Keywords: allyl palladium chloride dimer, methallyl, palladium, 50