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Continuous Synthesis and Purification by Coupling a Multistep Flow Reaction with Centrifugal Partition Chromatography
Author(s) -
Örkényi Róbert,
Éles János,
Faigl Ferenc,
Vincze Péter,
Prechl Anita,
Szakács Zoltán,
Kóti János,
Greiner István
Publication year - 2017
Publication title -
angewandte chemie
Language(s) - English
Resource type - Journals
eISSN - 1521-3757
pISSN - 0044-8249
DOI - 10.1002/ange.201703852
Subject(s) - chemistry , flow chemistry , adsorption , morpholine , chromatography , packed bed , partition (number theory) , high performance liquid chromatography , continuous flow , catalysis , column chromatography , organic chemistry , physics , mathematics , combinatorics , mechanics
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.