2516-96-3Relevant articles and documents
Advanced Real-Time Process Analytics for Multistep Synthesis in Continuous Flow**
Sagmeister, Peter,Lebl, René,Castillo, Ismael,Rehrl, Jakob,Kruisz, Julia,Sipek, Martin,Horn, Martin,Sacher, Stephan,Cantillo, David,Williams, Jason D.,Kappe, C. Oliver
, p. 8139 - 8148 (2021)
In multistep continuous flow chemistry, studying complex reaction mixtures in real time is a significant challenge, but provides an opportunity to enhance reaction understanding and control. We report the integration of four complementary process analytical technology tools (NMR, UV/Vis, IR and UHPLC) in the multistep synthesis of an active pharmaceutical ingredient, mesalazine. This synthetic route exploits flow processing for nitration, high temperature hydrolysis and hydrogenation reactions, as well as three inline separations. Advanced data analysis models were developed (indirect hard modeling, deep learning and partial least squares regression), to quantify the desired products, intermediates and impurities in real time, at multiple points along the synthetic pathway. The capabilities of the system have been demonstrated by operating both steady state and dynamic experiments and represents a significant step forward in data-driven continuous flow synthesis.
Synthesis method for (2-chloro-5-iodophenyl)(4-fluorophenyl)ketone
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Paragraph 0037; 0038, (2017/07/12)
The invention discloses a synthesis method for (2-chloro-5-iodophenyl)(4-fluorophenyl)ketone. According to the method, with cheap o-chlorobenzoic acid as a starting material, (2-chloro-5-iodophenyl)(4-fluorophenyl)ketone is obtained by nitration, Friedel-Crafts acylation and reduction and finally by Sandmeyer reaction for iodination. The materials used by the method are cheap and easy to obtain, and the method adopting Sandmeyer reaction for iodination can increase the iodine utilization rate, and has the characteristics of simplicity in operation, high yield, high purity and suitability for industrialized production. (The chemical formula is shown in the specification).
Method for synthesizing 2-chloro-5-nitrobenzoic acid through microchannel reactor
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Paragraph 0044-0047, (2017/08/29)
The invention provides a method for synthesizing 2-chloro-5-nitrobenzoic acid through a microchannel reactor. The method comprises the steps of dissolving a raw material o-chlorobenzoic acid into concentrated sulfuric acid to obtain a material 1, and entering a preheating module; adopting fuming nitric acid and the concentrated sulfuric acid as a material 2 and a material 3, and entering another preheating module; preheating the material 1, the material 2 and the material 3, entering a reaction module group for reacting, collecting effluent reaction liquid, processing to obtain a crude product, and refining to obtain the product 2-chloro-5-nitrobenzoic acid. According to the method provided by the invention, the reaction time is shortened to a few minutes to a few seconds, the production energy consumption is reduced, and the reaction efficiency is remarkably improved. High-efficient mass and heat transfer efficiency ensures the reaction temperature to maintain within a setting range, the possibilities of temperature out of control, temperature runaway and even sharp reaction overflow or explosion caused by over-high local concentration do not exist, the intrinsic safety problem of the nitration reaction is solved fundamentally, and the reaction yield and the product purity are remarkably improved.