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Continuous-Flow In-Line Solvent-Swap Crystallization of Vitamin D3.
Organic Process Research & Development ( IF 3.4 ) Pub Date : 2017-12-27 , DOI: 10.1021/acs.oprd.7b00351
Marc Escribà-Gelonch 1 , Volker Hessel 1 , Manuel C Maier 2 , Timothy Noël 1 , Maria Fernanda Neira d'Angelo 1 , Heidrun Gruber-Woelfler 2, 3
Affiliation  

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 D3. This configuration is suitable to be coupled to a new end-to-end continuous microflow synthesis of Vitamin D3. 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 D3 are directly obtained. Furthermore, the polymorphic form as well as crystals shape and size properties are described in this paper.

中文翻译:

维生素D3的连续流在线溶剂交换结晶。

提出了连续串联在线蒸发结晶。该方法包括在线溶剂交换步骤,该步骤适合于耦合到基于毛细管的冷却器上。作为概念验证,此设置在直接在线乙腈介导的维生素D3结晶中进行测试。这种配置适合与维生素D3的新的端到端连续微流合成相结合。通过此程序,维生素颗粒可以连续流动的方式结晶,并使用在线连续过滤步骤进行分离。在仅1分钟的冷却时间内运行一次,即可直接获得约50%(w / w)的维生素D3晶体。此外,本文还描述了多晶型物以及晶体的形状和尺寸特性。
更新日期:2018-01-17
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