Effect of Acetonitrile-Based Crystallization Conditions on the Crystal Quality of Vitamin D3

Heidrun Gruber-Woelfler*, Marc Escribà-Gelonch, Timothy Noël, Manuel C. Maier, Volker Hessel

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

Abstract

To design an integrated continuous crystallization setup that is directly coupled to a photochemical synthesis in flow, the crystallization of vitamin D3 was studied in detail. Because of the high solubility of the vitamin in the reaction solvent tert-butylmethyl ether, a solvent swap to acetonitrile was necessary. While other methods use a multistep procedure, with the proposed approach, crystalline vitamin D3 can be obtained within one crystallization step. The influence of crystallization parameters, such as the initial concentration of vitamin D3, stirring as well as cooling temperature, rate, and time, on the obtained results in terms of yield, crystal shape, polymorphism, and particle size distribution are discussed in detail.

Original languageEnglish
Pages (from-to)2016-2024
Number of pages9
JournalChemical Engineering & Technology
Volume40
Issue number11
DOIs
Publication statusPublished - 1 Nov 2017

Keywords

  • Crystallization
  • Polymorphism
  • Solubility
  • Vitamin D

Fields of Expertise

  • Advanced Materials Science

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