Continuous and scalable synthesis of a porous organic cage by twin screw extrusion (TSE)

被引：31

作者：

Egleston, Benjamin D. ^{[1
]}

Brand, Michael C. ^{[1
]}

Greenwell, Francesca ^{[1
]}

Briggs, Michael E. ^{[1
]}

James, Stuart L. ^{[2
]}

Cooper, Andrew, I ^{[1
]}

Crawford, Deborah E. ^{[3
]}

Greenaway, Rebecca L. ^{[1
,4
]}

机构：

[1] Univ Liverpool, Dept Chem & Mat Innovat Factory, 51 Oxford St, Liverpool L7 3NY, Merseyside, England

[2] Queens Univ Belfast, Sch Chem & Chem Engn, 39-123 Stranmillis Rd, Belfast BT9 5AG, Antrim, North Ireland

[3] Univ Bradford, Sch Chem & Biosci, Richmond Rd, Bradford BD7 1DP, W Yorkshire, England

[4] Imperial Coll London, Dept Chem, White City Campus,Wood Lane, London W12 0BZ, England

来源：

CHEMICAL SCIENCE | 2020年 / 11卷 / 25期

基金：

英国工程与自然科学研究理事会; 欧洲研究理事会;

关键词：

SOLVENT-FREE SYNTHESIS; MECHANOCHEMICAL SYNTHESIS; SELECTIVITY; SEPARATION;

D O I：

10.1039/d0sc01858a

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

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.

引用

页码：6582 / 6589

页数：8

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