Process for the isolation of crystalline 1,3- cyclohexanedione

Details Process for the isolation of crystalline 1,3- cyclohexanedione Process for the isolation of crystalline 1,3- cyclohexanedione

C - Chemistry, Metallurgy

07

C

167/327

C07C 49/403 (2006.01) C07C 45/45 (2006.01) C07C 45/81 (2006.01) C07C 45/83 (2006.01) C07D 309/32 (2006.01) C07D 315/00 (2006.01)

Patent

CA 1200558

Abstract of the Disclosure: The invention provides a process for the isolation of crystalline 1,3-cyclohexanedione from the crude product formed in the catalytic gaseous phase cycliza- tion of 5-oxohexanoic acid. Before or directly after condensation an auxiliary component consisting of at least one compound selected from the group consisting of cyclic hydrocarbons, chlorinated aliphatic hydrocar- bons and monoethers is added to the crude product, sub- sequently the mixture of crude product and auxiliary component is distilled under normal or reduced pressure until the reaction water is removed and the residual content of auxiliary component in the remaining concen- trate has attained a defined value, and the precipita- ted crystalline 1,3-cyclohexanedione is filtered off. Alternatively, the auxiliary component added may be di- stilled off substantially completely. In this case, ei- ther the same or another of the compounds or compound mixtures indicated as auxiliary component must be added subsequently to the remaining concentrate interspersed with crystals in order to obtain a substantially com- plete precipitation of the 1,3-cyclohexanedione in the form of crystals and formation of a filterable crystal pulp. Alternatively, the crude product may be heated af- ter condensation and the crude crystallized product ob- tained optionally after cooling be mixed with the auxi- liary component. The further work-up is as described above.

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