Journal
CHEMICAL SCIENCE
Volume 11, Issue 25, Pages 6582-6589Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/d0sc01858a
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Funding
- Engineering and Physical Sciences Research Council (EPSRC) [EP/R005710/1, EP/R005540/1]
- European Research Council under FP7, RobOT, ERC Grant [321156]
- Royal Society
- EPSRC [EP/R005710/1, EP/R005540/1] Funding Source: UKRI
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The continuous and scalable synthesis of a porous organic cage (CC3), obtained through a 10-component imine polycondensation between triformylbenzene and a vicinal diamine, was achieved using twin screw extrusion (TSE). Compared to both batch and flow syntheses, the use of TSE enabled the large scale synthesis ofCC3using minimal solvent and in short reaction times, with liquid-assisted grinding (LAG) also promoting window-to-window crystal packing to form a 3-D diamondoid pore network in the solid state. A new kinetically trapped [3+5] product was also observed alongside the formation of the targeted [4+6] cage species. Post-synthetic purification by Soxhlet extraction of the as-extruded 'technical grade' mixture ofCC3and [3+5] species rendered the material porous.
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