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Continuous synthesis of dolutegravir sodium crystals using liquid-gas heterogeneous microreactor

Chinese Chemical Letters 2023年第3期34卷 302-307页

作者： Wei Luo Fen Liu Yaohao Guo Junjie Qiu Jinrui Yan Shuangliang Zhao Bo Bao State Key Laboratory of Chemical Engineering and School of Chemical Engineering East China University of Science and TechnologyShanghai 200237China Guangxi Key Laboratory of Petrochemical Resource Processing and Process Intensification Technology and School of Chemistry and Chemical Engineering Guangxi UniversityNanning 530004China

In this work, a liquid-gas heterogeneous microreactor was developed for investigating continuous crystallization of dolutegravir sodium(DTG), as well as revealing reaction kinetics and mixing mechanism with 3-min data acquisition. The reaction kinetics models were established by visually recording the concentration variation of reactants over time in the microchannel via adding pH-sensitive fluorescent dye. The mixing intensification mechanism of liquid-gas flow was quantified through the fluorescent signal to indicate mixing process, demonstrating an outstanding mixing performance with a mixing time less than 0.1 s. Compared with batch crystallization, continuous synthesis of dolutegravir sodium using liquid-gas heterogenous microreactor optimizes crystal distribution size, and successfully modifies the crystal morphology in needle-like habit instead of rod-like habit. The microreactor continuous crystallization can run for 5 h without crystal blockage and achieve D90 of DTG less than 30 μm. This work provides a feasible approach for continuously synthesizing dolutegravir sodium, and can optimize the existing pharmaceutical crystallization.

关键词： Microreactor continuous crystallization dolutegravir sodium Reaction kinetics Mixing mechanism Crystal morphology Process operation

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