From Evaporative to Cooling Crystallisation: An Initial Co-Crystallisation Study of Cytosine and Its Fluorinated Derivative with 4-chloro-3,5-dinitrobenzoic Acid

Crystals

Kate Wittering¹  Josh King¹  Lynne H. Thomas¹ 

[1] Department of Chemistry, University of Bath, Bath, BA2 7AY, UK; E-Mails:

关键词: molecular complexes;    multi-component crystallisation;    continuous manufacturing and crystallisation;    cooling crystallisation;    process analytical technologies;    turbidity measurements;   

DOI  :  10.3390/cryst4020123

来源: mdpi

【 摘 要 】

Two new multi-component molecular complexes of cytosine and 5-fluorocytosine with 4-chloro-3,5-dinitrobenzoic acid are presented. Materials synthesis was achieved initially by evaporative crystallisation and the crystal structures determined. The process was then successfully transferred into a controlled small scale cooling crystallisation environment, with bulk samples shown to be representative of the multi-component product phase, by powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC) methods. Turbidity measurements are shown to be a valuable process analytical technology probe for characterising the initial stages of molecular complex formation in solution. The significance of these findings for scale-up of crystallisation of multi-component molecular materials and for future transfer into continuous cooling crystallisation is discussed.

【 授权许可】

CC BY   
© 2014 by the authors; licensee MDPI, Basel, Switzerland.