Microwave heating limitations

Today, a large body of work on microwave-assisted synthesis exists in the published and patent literature. Many review articles [8-20], several books [21-23], and information on the world-wide-web [24] already provide extensive coverage of the subject. The goal of the present book is to present carefully scrutinized, useful, and practical information for both beginners and advanced practitioners of microwave-assisted organic synthesis. Special emphasis is placed on concepts and chemical transformations that are of importance to medicinal chemists, and that have been reported in the most recent literature (2002-2004). The extensive literature survey is limited to reactions that have been performed using controlled microwave heating conditions, i.e., where dedicated microwave reactors for synthetic applications with adequate... 

Microwave heating is often applied to already known conventional thermal reactions in order to accelerate the reaction and therefore to reduce the overall process time. When developing completely new reactions, the initial experiments should preferably be performed only on a small scale applying moderately enhanced temperatures to avoid exceeding the operational limits of the instrument (temperature, pressure). Thus, single-mode reactors are highly applicable for method development and reaction optimization. 

The group of Lindau has demonstrated the effective O-alkylation of carboxylic acids using a polymer-supported O-methylisourea reagent [123], Under conventional conditions, complete esterifications were observed only after refluxing for several hours in tetrahydrofuran, and the acidic work-up required limited the scope of applicable substituents. In contrast, employing microwave heating led to complete esterifications within 15-20 min, with only 2 equivalents of the polymer-bound... 

The other limit is the problem of temperature measurements. Classical temperature sensors could be avoided in relation to power level. Hence, temperature measurements will be distorted by strong electric currents induced inside the metallic wires insuring connection of temperature sensor. The technological solution is the optical fiber thermometers [35-39]. However, measurements are limited below 250 °C. For higher values, surface temperature can be estimated by infrared camera or pyrometer [38, 40], However, due to volumic character of microwave heating, surface temperatures are often inferior to core temperatures. 

To use microwave heating in solid state synthesis, at least one component of the reaction mixture must absorb microwave radiation. The speed of the reaction process is then increased by both increasing the rate of the solid state reaction and by increasing the rate of diffusion, which, as we mentioned earlier, is often the rate-limiting step. 

This chapter is a non-comprehensive summary of the available papers where microwave dielectric heating has been used in combination with multi-component reactions. The examples highlight the fabulous possibilities that can be found in the cross-section of these technologies. The numbers of papers describing the combination are still limited, but nevertheless microwave heating will have an impact in the area and most certainly, we will see an increased number of publications and increased interest in the near future. 

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