C - Chemistry – Metallurgy – 07 – C
Patent
C - Chemistry, Metallurgy
07
C
260/486.7
C07C 67/36 (2006.01) C07C 69/34 (2006.01)
Patent
CA 1127179
O.Z. 0050/033918 Abstract of the disclosure: A process for the pre- paration of butanedicarboxylic acid esters, wherein a) an aqueous cobalt salt solution is treated, at from 50 to 200°C and under a pressure of from 50 to 500 bar, with excess carbon monoxide and hydrogen in the presence of active charcoal which has been 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, con- taining cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon monoxide and excess C1-C4-alkanol in the presence of from 0.5 to 2 moles, per mole of butadiene, of a tert- iary nitrogen base having a pKa of from 3 to 11, at from 80 to 150°C under a pressure of from 300 to 2,000 bar, 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 penten- oic acid ester remaining in the reaction mixture is reacted with carbon monoxide and excess C1-C4-alkanol at from 140 to 200°C and under a pressure of from 100 to 400 bar in the presence of the amounts of cobalt carbonyl and tertiary nitrogen base contained in the reaction mix- ture, O.Z. 0050/033918 e) the reaction mixture containing cobalt catalyst, butanedicarboxylic acid esters, alkanols, tertiary nitro- gen base, pentenoic acid esters and by-products 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 iso- lated by distillation, and an aqueous phase, and f) the aqueous phase is extracted with C1-C4-alkyl esters of C1-C5-alkanecarboxylic acids and/or alkene- carboxylic acids, the phases are separated, and the aqueous phase thus obtained is freed from alkanols and tertiary nitrogen base by distilling these off and is recycled to stage a).
351999
Kummer Rudolf
Schneider Heinz-Walter
Taglieber Volker
Weiss Franz-Josef
Basf Aktiengesellschaft
Robic Robic & Associes/associates
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