butyllithium; CH2Cl2 in tetrahydrofuran; diethyl ether; benzene Li(PyPhCH) in THF (prepd. in situ) added dropwise over 30 min to stirred suspn. of PdCl2(γmpy) in ether at -80°C under N2; warmed to room temp.; benzene added; soln. 1 h heated to 60°C (ether distd.); cooled deep red soln. hydrolysed; organic phase isolated, filtered, dried over MgSO4, reduced to dryness in vac.; red orange gum extd. with hot hexane; remaining gum dissolved in CH2Cl2; acetone added; orange crystals sepd. by slow evapn. (20 h); elem. anal.;

butyllithium in tetrahydrofuran; diethyl ether; benzene Li(PyPhCH) in THF (prepd. in situ) added dropwise over 30 min to stirred suspn. of PdCl2(γmpy) in ether at -80°C under N2; warmed to room temp.; benzene added; soln. 1 h heated to 60°C (ether distd.); cooled deep red soln. hydrolysed; org. phase isolated, dried, reduced to dryness; red orange gum chromd. on SiO2 (Et acetate/CHCl3); first orange fraction Pd((PyPhC)C(Me)O)2 recrystd. (acetone/CH2Cl2); (Pd(PyPhCH)(γmpy)Cl)2 isolable from retaining material on column; elem. anal.;