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On the Effect of Secondary Nucleation on Deracemization through Temperature Cycles.
Chemistry - A European Journal ( IF 4.3 ) Pub Date : 2020-01-22 , DOI: 10.1002/chem.201904239
Fabio Cameli 1 , Joop H Ter Horst 2 , René R E Steendam 3 , Christos Xiouras 4 , Georgios D Stefanidis 1
Affiliation  

Herein, the pivotal role of secondary nucleation in a crystallization-enhanced deracemization process is reported. During this process, complete and rapid deracemization of chiral conglomerate crystals of an isoindolinone is attained through fast microwave-assisted temperature cycling. A parametric study of the main factors that affect the occurrence of secondary nucleation in this process, namely agitation rate, suspension density, and solute supersaturation, confirms that an enhanced stereoselective secondary nucleation rate maximizes the deracemization rate. Analysis of the system during a single temperature cycle showed that, although stereoselective particle production during the crystallization stage leads to enantiomeric enrichment, undesired kinetic dissolution of smaller particles of the preferred enantiomer occurs during the dissolution step. Therefore, secondary nucleation is crucial for the enhancement of deracemization through temperature cycles and as such should be considered in further design and optimization of this process, as well as in other temperature cycling processes commonly applied in particle engineering.

中文翻译:

关于二次成核对温度循环中脱氮作用的影响。

在此,报道了二次成核在结晶增强的脱硝过程中的关键作用。在此过程中,通过快速的微波辅助温度循环,可以实现异吲哚满酮的手性团聚体晶体的完全,快速脱硝。对这一过程中影响次生成核的主要因素进行参数研究,即搅拌速率,悬浮液密度和溶质过饱和,证实增强的立体选择性次生成核速率可以最大程度地提高脱团率。在一个温度周期内对系统的分析表明,尽管在结晶阶段产生立体选择性颗粒会导致对映体富集,优选的对映异构体的较小颗粒的不希望的动力学溶解在溶解步骤中发生。因此,二次成核对于通过温度循环增强脱硝作用至关重要,因此在进一步设计和优化此过程以及在粒子工程中通常使用的其他温度循环过程中应考虑到二次成核。
更新日期:2020-01-23
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