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Co-crystallisation of α,ω-dicarboxylic acids with nicotinamide and isonicotinamide

Voguri, Raja Sekhar (2010)
M.Res. thesis, University of Birmingham.

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Abstract

Pharmaceutical co-crystallisation is an alternative and potentially reliable method to manipulate physical properties of API’s via supramolecular synthesis. A number of binary co-crystals were synthesised using different solvents, different stoichiometric ratios (ratio of starting materials) and different methods of synthesis (solvent-mediated crystallisation, solvent-drop grinding and neat grinding), with a view to investigate solvent and stoichiometric effects on the materials formed. Selected α,ω-alkanedicarboxylic acids (HOOC-(CH\(_2\))\(_{n-}\)COOH) were crystallised with nicotinamide for n = 0, 1, 2, 4, 5, 6, 7 and isonicotinamide for n = 5, 6, 7 yielding 12 new solid materials. The melting point of the starting materials and new products are determined and analysed, and the new crystalline materials characterised using NMR, FTIR, powder X-ray diffraction data (PXRD) and single X-ray diffraction data (SXRD). For azelaic acid : nicotinamide (1:1), structure solution was carried out using powder X-ray diffraction data and the direct space methods are applied through differential evolution (DE) approach. The crystal structure of adipic acid : nicotinamide (1:2) was solved using single crystal X-ray diffraction. The crystal structures of both, display strong O-H….N(pyridine), O-H\(^{….}\)O=C and N-H\(^{….}\)O=C intermolecular bonds. Other new materials formed were oxalic acid:nicotinamide (1:1 and 1:2), malonic acid : nicotinamide (1:1 and 1:2), succinic acid : nicotinamide (1:1), pimelic acid : nicotinamide (1:1), suberic acid : nicotinamide (1:1), azelaic acid : nicotinamide (1:1), pimelic acid : isonicotinamide (1:1), suberic acid : isonicotinamide (1:1 and 1:2) and azelaic acid : isonicotinamide (1:1), but these were not fully characterised by X-diffraction.

Type of Work:M.Res. thesis.
Supervisor(s):Tremayne, Maryjane
School/Faculty:Colleges (2008 onwards) > College of Engineering & Physical Sciences
Department:School of Chemistry
Subjects:QD Chemistry
Institution:University of Birmingham
ID Code:1149
This unpublished thesis/dissertation is copyright of the author and/or third parties. The intellectual property rights of the author or third parties in respect of this work are as defined by The Copyright Designs and Patents Act 1988 or as modified by any successor legislation. Any use made of information contained in this thesis/dissertation must be in accordance with that legislation and must be properly acknowledged. Further distribution or reproduction in any format is prohibited without the permission of the copyright holder.
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