Manufacture of butanedicarboxylic acid esters

C - Chemistry – Metallurgy – 07 – C

Patent

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260/486.7

C07C 69/44 (2006.01)

Patent

CA 1115290

Abstract of the disclosure: A process for the manufacture of butanedicarboxylic acid esters, wherein a) an aqueous cobalt salt solution is treated with carbon monoxide and hydrogen in the presence of active charcoal, b) the resulting aqueous solution is extracted with buta- diene or with a hydrocarbon mixture containing butadiene, c) the butadiene, or butadiene/hydrocarbon mixture, con- taining cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon mon- oxide and an excess of an alkanol of 1 to 4 carbon atoms in the presence of a tertiary nitrogen base, d) the tertiary nitrogen bases contained in the resulting reaction mixture are removed from the latter to the extent of leaving from 0.1 to 0.3 mole per mole of pen- tenoic acid ester, excess hydrocarbons are also removed, the pentenoic acid ester remaining in the reaction mix- ture is reacted with carbon monoxide and an alkanol of 1 to 4 carbon atoms, and thereafter excess alkanol and free nitrogen base are distilled off and e) the residual reaction mixture, containing cobalt cata- lysts, butanedicarboxylic acids and by-products is treated with an oxidizing agent in an aqueous acid medium and the mixture is separated into an organic phase, from which butanedicarboxylic acid esters are isolated by distillation, and an aqueous phase containing cobalt salts, which phase is extracted with a water-immiscible solvent.

310829

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