Quality By Design Symposium 2019:

Online Monitoring and Control of Mechanosynthesis

26 March 2019, De Montfort University, Leicester, UK

John Mack, Darren Whitaker - Perceptive Engineering

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7th Quality by Design Symposium

How Can Industry Better Support National Healthcare Systems?

This event will bring together academics, regulators and industrial experts, to share academic research aligned to the QbD agenda as well as progress in ‘real life’ QbD implementation.


Continuous Solid-State Mechanochemical Diels-Alder Reaction of Anthracene and Maleic Anhydride with Inline Uv-Vis Spectrophotometry Process Monitoring

Rahamatullah Shaikh1,Darren Whitaker2, Dan Palmer3, Ahmad B. Albadarin4, Denise M. Croker5 & Gavin M. Walker5

Recently, demand for greener and more environmentally sustainable processes has led to increased attention on mechanochemical process. Mechanochemical synthesis is one in which solid reactants are vigorously ground (milling or grinding) together with minimal or even no solvent. Mechanochemical synthesis is applied to a variety of different compounds such as inorganic and organic compounds. Diels-Alder reaction is a significant method in producing new pharmaceutical and chemical molecules. Solid-state Diels-Alder reactions have been successfully performed in a ball mill however, their use is limited due to the ineffective milling temperature control, long milling times and scale up issues. Twin screw extrusion has recently been used for discovery of new or improved reactivity and products such as coordination polymers, metal-organic frameworks, various organic molecules and pharmaceutical cocrystals. Here, for the first time, we report on continuous solid-state mechanochemical Diels-Alder reaction of Anthracene and Maleic Anhydride and to real-time UV-Vis spectrophotometry process monitoring. Reactions were carried out at various key extrusion processing parameters and influence complete conversion to the product has been studied. The product formation was investigated with various techniques, including 1HNMR spectroscopy, PXRD, thermal analysis and microscopy. Furthermore, it was demonstrated that the inline UV-Vis spectrophotometry analysis provided additional information on mechanistic understanding of process development.

1 Department of Chemical Sciences, Bernal Institute, University of Limerick, Limerick, Ireland; 2 Perceptive Engineering Limited, UK
3 Colvistec GMBH, Germany; 4Pharmaceutical Manufacturing Technology (PMTC), Bernal Institute, University of Limerick, Ireland
5Synthesis & Solid State Pharmaceutical Centre (SSPC), Bernal Institute, University of Limerick, Ireland

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