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When tetracarbonylhydridocobalt reacted with dimethyl fumarate at 10-degrees-C, tetracarbonyl[1,2-bis(methoxycarbonyl)ethyl]cobalt was formed and isolated in 65% yield. The rate of the accompanying carbon monoxide uptake was found to be 0.5 order with respect to Co2(CO)8. Tetracarbonyl-alpha-hydroxyalkylcobalts were prepared by the reactions Of tetracarbonylhydridocobalt with formaldehyde, pivalaldehyde, glyoxal, ethyl glyoxylate, and crotonaldehyde between -40 and -79-degrees-C and characterized partly in the form of their silylated derivatives by IR and NMR spectroscopy. 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