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Crystals 2014, 4(2), 123-140; doi:10.3390/cryst4020123
Article

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

1,2
,
1
,
1
 and
1,2,*
1 Department of Chemistry, University of Bath, Bath, BA2 7AY, UK 2 Engineering and Physical Sciences Research Council (EPSRC) Centre for Continuous Manufacturing and Crystallisation (CMAC), University of Bath, Bath, BA2 7AY, UK
* Author to whom correspondence should be addressed.
Received: 20 December 2013 / Revised: 21 May 2014 / Accepted: 29 May 2014 / Published: 11 June 2014
(This article belongs to the Special Issue Crystallisation Control)

Abstract

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.
Keywords: molecular complexes; multi-component crystallisation; continuous manufacturing and crystallisation; cooling crystallisation; process analytical technologies; turbidity measurements molecular complexes; multi-component crystallisation; continuous manufacturing and crystallisation; cooling crystallisation; process analytical technologies; turbidity measurements
This is an open access article distributed under the Creative Commons Attribution License (CC BY 3.0).
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Wittering, K.; King, J.; Thomas, L.H.; Wilson, C.C. From Evaporative to Cooling Crystallisation: An Initial Co-Crystallisation Study of Cytosine and Its Fluorinated Derivative with 4-chloro-3,5-dinitrobenzoic Acid. Crystals 2014, 4, 123-140.

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