Chloro methyl bis triphenylphosphine palladium II

PdClMe(tmeda) 4- 2PPh3 -+ frans-PdClMe(PPh3)2 + tmeda 

In a 25-mL, round-bottomed flask, PPh3 (0.25 g, 0.95 mmol) is added to a solution of PdClMe(tmeda) (0.12g, 0.44 mmol) in dichloromethane (10 mL). A precipitate is formed within a few minutes, and after stirring for 45 min the solvent is removed in a vacuum and the white product is washed with hexane (3xl0mL) and dried in vacuo (0.29g, 97%). HNMR in CDC13 81.10 (m, 12H), 7.39 (m, 18H) [C6H5], -0.01 (t,3H, JH-p 6 Hz) [PdMe]. 31P H NMR in CDC13 8 30.9. 

SYNTHESIS OF PPh3 AND dppf COMPLEXES FROM PdXMe (tmeda) 

Using methods K and L, the following complexes can be obtained, with yields in parentheses PdMe2(bpy) (86%), PdMe2(dppf) (85%), 

PdClMe(tmeda) -I- 2 PPh3 - trans-PdClMe(PPh3)2 -I- tmeda 

The analogous complexes PdBrMe(bpy) and PdlMe(bpy) can be prepared in a similar way to give yields of 61 and 41%, respectively. 

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