Ligand Exchange with Nickel O Complexes

5cheme 56 Preparation of Bis(methyl acrylate)(pyridine)nickel(0)P 21 

To NiClj SHjO (4.7 g, 20 mmol), methyl acrylate (5.0 ml, 55 mmol), and p5Tidine (5.0 ml, 61 mmol) in THF (50 ml) was added Zn powder (5.0 g, 76 mmol). The suspension was heated to 60 °C, and the oil bath was removed. After 2 h the mixture was filtered, and the solid residue was washed with THF (3x15 ml). After removal of the solvent in vacuo, extraction with Et20 (50 mL) left behind the insoluble zinc salts. Filtration and evaporation of the extract in vacuo gave a red oil which was treated with hexane to dissolve the excess pyridine and methyl acrylate. The hexane layer was discarded, and the residual oil was dissolved in EtaO (50 mL). Cooling to -18 °C afforded 69 as a pale orange powder yield 4.3 g (70%) mp 80 °C (dec). 

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