Continuous-Flow In-Line Solvent-Swap Crystallization of Vitamin D3

Marc Escribà-Gelonch, Volker Hessel, Manuel C. Maier, Timothy Noël, Maria Fernanda Neira D'Angelo, Heidrun Gruber-Woelfler

Research output: Contribution to journalArticleAcademicpeer-review

6 Citations (Scopus)
121 Downloads (Pure)

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.

Original languageEnglish
Pages (from-to)178-189
Number of pages12
JournalOrganic Process Research & Development
Volume22
Issue number2
DOIs
Publication statusPublished - 1 Feb 2018

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