| 摘要 |
A process for the preparation of butanedicarboxylic acid esters, wherein (a) an aqueous cobalt salt solution is treated with excess carbon monoxide and hydrogen in the presence of active charcoal laden with cobalt carbonyl, (b) the resulting aqueous solution of cobalt carbonyl hydride is extracted with butadiene or a butadiene containing hydrocarbon mixture and the aqueous phase is separated off, (c) the butadiene, or butadiene/hydrocarbon mixture, containing cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon monoxide and excess C1-C4-alkanol in the presence of a tertiary nitrogen base, (d) the resulting reaction mixture is freed from the tertiary nitrogen base contained therein, down to a content of from 0.1 to 0.3 mole per mole of pentenoic acid ester, and from excess hydrocarbons, and the pentenoic acid ester remaining in the reaction mixture is reacted with carbon monoxide and excess C1-C4-alkanol in the presence of the cobalt carbonyl and tertiary nitrogen base contained in the reaction mixture, (e) the reaction mixture is treated with an oxidizing agent in the presence of the aqueous acid solution which has been separated off in stage (b), and the mixture is separated into an organic phase, from which butanedicarboxylic acid esters are isolated by distillation, and an aqueous phase, and (f) the aqueous phase is extracted with water-immiscible solvents, the phases are separated, and the resulting aqueous phase is freed from alkanols and tertiary nitrogen base and is recycled to stage (a).
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