Co-reporter:Duncan L. Browne, Marcus Baumann, Bashir H. Harji, Ian R. Baxendale, and Steven V. Ley
Organic Letters 2011 Volume 13(Issue 13) pp:3312-3315
Publication Date(Web):May 26, 2011
DOI:10.1021/ol2010006
A new machine for conducting continuous flow processes at low temperatures on a laboratory scale is reported. The use of this cryogenic flow reactor has been demonstrated by the preparation of a variety of (hetero)aromatic boronic acids and esters via lithium halogen exchange chemistry. Furthermore, scale-up of the reaction conditions not only demonstrates the application of this device for the preparation of useful building blocks but also combines the ability to process n-butyllithium directly through pump heads attached to the unit.
Co-reporter:Duncan L. Browne, Benjamin J. Deadman, Robert Ashe, Ian R. Baxendale, and Steven V. Ley
Organic Process Research & Development 2011 Volume 15(Issue 3) pp:693-697
Publication Date(Web):March 9, 2011
DOI:10.1021/op2000223
A general method for the continuous processing of suspensions and particulates is reported. A commercially available agitating cell reactor which uses a transverse mixing motion to maintain solids in suspension has been successfully applied to a salt-forming reaction. The flow device delivered 208 g of N-iodomorpholinium hydroiodide salt over a 9-h period (equating to 3.88 kg/week) under optimized conditions. The reactor is suitable for the medium-scale (5 kg) processing of solid-forming reactions and appears to offer the potential for a variety of more complex applications.