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Type: Journal article
Title: Continuous-flow in-line solvent-swap crystallization of vitamin D₃
Other Titles: Continuous-flow in-line solvent-swap crystallization of vitamin D(3)
Author: Escribà-Gelonch, M.
Hessel, V.
Maier, M.
Noël, T.
Neira D'Angelo, M.
Gruber-Woelfler, H.
Citation: Organic Process Research and Development, 2018; 22(2):178-189
Publisher: ACS Publications
Issue Date: 2018
ISSN: 1083-6160
Statement of
Marc Escribà-Gelonch, Volker Hessel, Manuel C. Maier, Timothy Noël, Maria Fernanda Neira d’Angelo and Heidrun Gruber-Woelfler
Abstract: 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.
Rights: © 2017 American Chemical Society. ACS AuthorChoice - This is an open access article published under a Creative Commons Non-Commercial No Derivative Works (CC-BY-NC-ND) Attribution License, which permits copying and redistribution of the article, and creation of adaptations, all for non-commercial purposes.
DOI: 10.1021/acs.oprd.7b00351
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Appears in Collections:Aurora harvest 3
Chemistry publications

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