Electroorganic synthesis in microreactors

Aziz, Tamsila Nayyar

April 2009

Thesis or dissertation

© 2009 Tamsila Nayyar Aziz. All rights reserved. No part of this publication may be reproduced without the written permission of the copyright holder.

At present, description of applications, using electrochemical micro reactor are rare. Such techniques are extremely desirable to pharmaceutical companies who are interested in the high throughput synthesis of combinatorial libraries for pharmaceutical evaluation. Furthermore, techniques such as electrochemical synthesis may be used to prepare chemicals, which are difficult to prepare by conventional techniques.

The main aim of this research project was to identify any unique control, over electrochemical organic synthesis, that micro reactors offer, and the modification of methods to gain chemical and practical advantages. These advantages come from the close control that exists between flow, concentration and thermal properties with a diffusion limited small volume system.

The project involved investigation of certain factors, such as concentration of reacting species, the current limitations, and process flexibility of electro organic synthesis, in micro reactors. To investigate these factors, a versatile reaction for organic synthesis Kolbe electrolysis is selected, without using an electrolyte, in order to benefit from the quick separation and purification of products. The anodic oxidation of carboxylic acids produces alkanes by dimerization of the radicals generated at the anode.

To investigate this reaction, in a micro reactor environment, several batch cell/flow system arrangements were employed in order to achieve the optimum yields. Once a set of conditions giving optimum yield is established, the system will be applicable to the electrochemical synthesis, and to develop novel methods to optimize various reactions and prepare reactive intermediates in situ.

Department of Chemistry, The University of Hull
Watts, Paul, 1974-; Haswell, S. J. (Stephen John), 1954-
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