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连续流反应与离心分配色谱耦合法的多步合成与纯化。

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

机构信息

Department of Organic Chemistry and Technology, Budapest University of Technology and Economics, Budafoki út 8., 1111, Budapest, Hungary.

Gedeon Richter Plc., Gyömrői út 19-21., 1103, Budapest, Hungary.

出版信息

Angew Chem Int Ed Engl. 2017 Jul 17;56(30):8742-8745. doi: 10.1002/anie.201703852. Epub 2017 Jun 19.

DOI:10.1002/anie.201703852
PMID:28548374
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5519935/
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.

摘要

连续流多步合成与准连续最终产物纯化相结合,可从粗反应混合物中生产出纯产物。在 2,4-二氟硝基苯与吗啉的亲核芳香取代反应,然后进行多相催化氢化反应中,通过将流反应器序列与多双模式(MDM)离心分配色谱(CPC)设备相耦合,可以将所需的单取代产物连续地从共反应物和副产物中分离出来,纯度超过 99%。与 HPLC 相比,这种纯化技术具有许多优势,例如更高的分辨率,不需要更换柱子或回收硅胶,并且不会发生不可逆吸附。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/0ec9d8594962/ANIE-56-8742-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/e4e456da4297/ANIE-56-8742-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/dcb6a6711712/ANIE-56-8742-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/0ec9d8594962/ANIE-56-8742-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/e4e456da4297/ANIE-56-8742-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/dcb6a6711712/ANIE-56-8742-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f99f/5519935/0ec9d8594962/ANIE-56-8742-g003.jpg

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