Escribà-Gelonch Marc, Hessel Volker, Maier Manuel C, Noël Timothy, Neira d'Angelo Maria Fernanda, Gruber-Woelfler Heidrun
Eindhoven University of Technology, Department of Chemical Engineering and Chemistry, De Rondom 70, 5612 AP Eindhoven, The Netherlands.
Graz University of Technology, Institute of Process and Particle Engineering, NAWI Graz, Inffeldgasse 13, 8010 Graz, Austria.
Org Process Res Dev. 2018 Feb 16;22(2):178-189. doi: 10.1021/acs.oprd.7b00351. Epub 2017 Dec 27.
A continuous tandem in-line evaporation-crystallization is presented. The process includes an in-line solvent-swap step, suitable to be coupled to a capillary based cooler. As a proof of concept, this setup is tested in a direct in-line acetonitrile mediated crystallization of Vitamin D. This configuration is suitable to be coupled to a new end-to-end continuous microflow synthesis of Vitamin D. By this procedure, vitamin particles can be crystallized in continuous flow and isolated using an in-line continuous filtration step. In one run in just 1 min of cooling time, ∼50% (w/w) crystals of Vitamin D are directly obtained. Furthermore, the polymorphic form as well as crystals shape and size properties are described in this paper.
本文提出了一种连续串联式在线蒸发-结晶方法。该过程包括一个在线溶剂交换步骤，适用于与基于毛细管的冷却器相连。作为概念验证，此装置在维生素D的直接在线乙腈介导结晶中进行了测试。这种配置适用于与新的维生素D端到端连续微流合成方法相结合。通过该程序，维生素颗粒可以在连续流动中结晶，并使用在线连续过滤步骤进行分离。在仅1分钟冷却时间的一次运行中，可直接获得约50%（w/w）的维生素D晶体。此外，本文还描述了多晶型以及晶体的形状和尺寸特性。
