Rehman Ghufran Ur, Vetter Thomas, Martin Philip A
Department of Chemical Engineering, University of Manchester, Manchester M13 9PL, U.K.
Cryst Growth Des. 2023 Jul 10;23(8):5428-5436. doi: 10.1021/acs.cgd.2c01138. eCollection 2023 Aug 2.
Chiral compounds can exist as pairs of nonsuperimposable stereoisomers (enantiomers) possessing the same physical properties but interacting differently with biological systems. This makes them interesting materials to be explored by the pharmaceutical and food industries. In this study, to obtain pure enantiomers from their conglomerates, a method that involves using a two-vessel system for deracemization of -(2-methylbenzylidene) phenylglycine amide (NMPA) was developed. In this method, a suspension was transferred with a pulsating pumping profile between two inter-connected stirred vessels that were set at constant temperatures. As the suspension was exposed to more rapid changes in temperature, it resulted in the speeding up of the process and thus enhancing productivity in comparison to a single vessel system. The results confirmed successful deracemization of NMPA. A modified pumping profile and tubing design eliminated the issue of clogging of the transfer tubes and ensured effective suspension transfer for longer durations. Operating parameters, such as initial enantiomeric excess, vessel residence time, and suspension density were also investigated. In this method, optimization of residence time was necessary to enhance the efficiency of the process further. Results confirmed that this methodology has the potential to be more adaptable and scalable as it involved no mechanical attrition.
手性化合物可以以一对不可重叠的立体异构体（对映体）形式存在，它们具有相同的物理性质，但与生物系统的相互作用不同。这使得它们成为制药和食品行业值得探索的有趣材料。在本研究中，为了从其聚集体中获得纯对映体，开发了一种使用双容器系统对α-(2-甲基亚苄基)苯甘氨酸酰胺（NMPA）进行外消旋化的方法。在该方法中，悬浮液以脉动泵送曲线在两个相互连接且设定为恒定温度的搅拌容器之间转移。由于悬浮液暴露于更快速的温度变化中，与单容器系统相比，这导致过程加速，从而提高了生产率。结果证实了NMPA的外消旋化成功。改进的泵送曲线和管道设计消除了传输管堵塞的问题，并确保了更长时间的有效悬浮液转移。还研究了操作参数，如初始对映体过量、容器停留时间和悬浮液密度。在该方法中，优化停留时间对于进一步提高过程效率是必要的。结果证实，该方法具有更大的适应性和可扩展性潜力，因为它不涉及机械磨损。
