Chemical Reactor Development: From Laboratory Synthesis to Industrial Production
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Microwave reactors at production scale
A range of pharmaceutically relevant reactions were investigated for scale-up in a kilo-lab environment using a commercial batch microwave reactor. Typical scale-up issues are discussed, taking into account the specific limitations of microwave heating in large-scale experiments.
Examples of scale-up from 15 mL to 1 L are presented and demonstrate that the synthesis of compounds on greater than g scale is feasible in one batch. Aided by this new technology reaction times have been significantly reduced and the productivity of our scale-up laboratory has been enhanced. Production rates of several hundred grams per day were achieved using microwave technology. The article concludes with a brief discussion of advantages and disadvantages of this type of batch microwave reactor.
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Rebrov, Jan Meuldijk, Lumbertus A. Hulshof, Volker Hessel, and Jaap C. DOI: Neal G. Using Continuous Processes to Increase Production. Moseley, Alexander Stadler, and C. The current reactor specification is shown in Table 1. Safety features include cut-offs on high temperature and pressure with bursting discs before and after the microwave-heated section.
The waveguide is flooded with nitrogen during operation and will contain the reactor contents in the case of failure. The waveguide is further surrounded by a safety cabinet, which must be closed for operation and the reactor assembly surrounded by an extracted fume hood. The first such reactor was built as a homogeneous reactor to prove the concept that heating a continuous chemical reaction by microwave energy was possible. A Hantsch dihydropyridine synthesis was chosen as the test reaction because these reactions are known to work well under microwave heating but also since suitable quantities of the starting materials were available on-site Figure 2.
In total, 7. Following this success, the configuration of the CaMWave KiloLAB reactor was changed with the addition of a custom pressure control system that would allow the handling of slurries and suspensions. A heterogeneously-catalysed Suzuki test reaction was chosen as again these reactions are known to proceed well under microwave heating Figure 3.
It was subsequently discovered that only 30s was needed to give the same yield and purity, and potentially the reaction could go even faster. A further feed vessel was added to enable two streams to be simultaneously fed rather than having to pre-mix all the reaction components.
An additional receiver vessel was also added, such that the two receivers can operate independently, allowing one to be emptied while the other continues to collect product. With this versatility in place, the reactor's potential as a viable manufacturing option was tested.
The reactor was operated continuously for 32hrs giving This is the longest microwave-enabled reaction as a single run, published to date, which corresponds to an impressive 5m t. The reactor can undertake most reported MAOS and Cambrex is using the reactor to synthesise early kilograms of material for development and scale-up projects.
Palladium-catalysed reactions have been studied in depth along with nucleophilic substitutions and alkylations with long batch reaction times. The high temperatures achieved with the reactor ensure very fast reactions. No new impurities have been observed to date, by either the high temperature or the switch to continuous-flow. In fact, impurities are usually greatly reduced such that downstream purification can be minimised or avoided. Metal catalyst loadings can easily and often be dramatically reduced under microwave heating. Usually at least one order of magnitude reduction can be achieved.