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Continuous Synthesis and Purification by Coupling a Multistep Flow Reaction with Centrifugal Partition Chromatography.

ABSTRACT: Continuous-flow multistep synthesis is combined with quasi-continuous final-product purification to produce pure products from crude reaction mixtures. In the nucleophilic aromatic substitution of 2,4-difluoronitrobenzene with morpholine followed by a heterogeneous catalytic hydrogenation, the desired monosubstituted product can be continuously separated from the co- and by-products in a purity of over 99 % by coupling a flow reactor sequence to a multiple dual-mode (MDM) centrifugal partition chromatography (CPC) device. This purification technique has many advantages over HPLC, such as higher resolution and no need for column replacement or silica recycling, and it does not suffer from irreversible adsorption.

SUBMITTER: Orkenyi R

PROVIDER: S-EPMC5519935 | biostudies-literature | 2017 Jul

REPOSITORIES: biostudies-literature

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Continuous Synthesis and Purification by Coupling a Multistep Flow Reaction with Centrifugal Partition Chromatography.

Örkényi Róbert R Éles János J Faigl Ferenc F Vincze Péter P Prechl Anita A Szakács Zoltán Z Kóti János J Greiner István I

Angewandte Chemie (International ed. in English) 20170619 30

Continuous-flow multistep synthesis is combined with quasi-continuous final-product purification to produce pure products from crude reaction mixtures. In the nucleophilic aromatic substitution of 2,4-difluoronitrobenzene with morpholine followed by a heterogeneous catalytic hydrogenation, the desired monosubstituted product can be continuously separated from the co- and by-products in a purity of over 99 % by coupling a flow reactor sequence to a multiple dual-mode (MDM) centrifugal partition c ...[more]

PMID: 28548374

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