Treatment of W(CO)6 with vinyllithium followed by Me3OBF4 in the presence of H2O produced (CO)5W[C(OCH3)CHCH2] (1) (25-30%) and (CO)5W[C(OCH3)-(η-CHCH2)]W(CO)5 (2) (20-30%). Complex 1 reacted with (CO)5W · THF to give W2(CO)9[μ-μ1,η3-C(OCH3)CHCH2] (3) (61%). Heating 2 to 45°C in toluene produced 3 (65%) which could be converted back to 2 upon treatment with CO. Complex 1 reacte with D2O in benzene-d6 to afford 2 and methyl propionate-2,3-d2 (4). A new route to 1 was developed from C(CO)6 in an overall yield of 40% using (CO)5W[C(O)CHCH2]NME4 (8) as an intermediate.
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We wish to thank the donors of the Petroleum Research Fund, administered by the American Chemical Society and the Research Corporation for partial support of this research.