Translating solid state organic synthesis from a mixer mill to a continuous twin screw extruder

被引：65

作者：

Cao, Qun ^{[1
]}

Howard, Joseph L. ^{[1
]}

Crawford, Deborah E. ^{[2
]}

James, Stuart L. ^{[2
]}

Browne, Duncan L. ^{[1
]}

机构：

[1] Cardiff Univ, Sch Chem, Main Bldg,Pk Pl, Cardiff CF10 3AT, S Glam, Wales

[2] Queens Univ Belfast, Sch Chem & Chem Engn, David Keir Bldg, Belfast BT9 5AG, Antrim, North Ireland

来源：

GREEN CHEMISTRY | 2018年 / 20卷 / 19期

基金：

英国工程与自然科学研究理事会;

关键词：

PHARMACEUTICAL CO-CRYSTALS; MECHANOCHEMICAL SYNTHESIS; BALL MILLS; SOLVENT; FRAMEWORKS; EXTRUSION; POLYMORPH; EFFICIENT; LIQUID; SCALE;

D O I：

10.1039/c8gc02036a

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

A study on the translation of a solid-state synthetic reaction from a mechanochemical mixer-mill to a continuous twin-screw extruder is discussed herein. The study highlights some considerations to be made and parameters to be tested in the context of a model fluorination reaction, which is the first organic fluorination to be attempted using extrusion. Upon optimization, which features the first use of grinding auxiliary solids to enable effective synthetic extrusion, the difluorination reaction was successfully translated to the extruder, leading to a 100-fold improvement in Space Time Yield (STY); 29 kg m(-3) day(-1) in a mixer mill to 3395 kg m(-3) day(-1) in a twin screw extruder.

引用

页码：4443 / 4447

页数：5

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