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An Inexpensive Adaptation of a Commercial Microwave Reactor for Solid Phase Peptide Synthesis
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Scale-up in microwave-accelerated organic synthesis.

H Lehmann1

  • 1Discovery Technologies/Preparation Laboratories, Novartis Institute for Biomedical Research, Klybeckstrasse 191, 4002 Basel, Switzerland. hansjoerg.lehmann@novartis.com

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Scaling up microwave-assisted organic chemistry is feasible, with reduced reaction times and improved yields. However, current large-scale microwave systems have limited vessel sizes for kilo-lab operations.

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Area of Science:

  • Organic Chemistry
  • Chemical Engineering
  • Process Chemistry

Background:

  • Microwave-assisted organic chemistry is widely used on a small scale.
  • Efficient application of microwave technology for large-scale preparations (kilo lab) remains underdeveloped.

Purpose of the Study:

  • To investigate the scalability of microwave technology for larger-scale organic synthesis.
  • To evaluate the strengths and weaknesses of different large-scale microwave systems for scale-up.

Main Methods:

  • Evaluation of two different large-scale microwave systems.
  • Focus on temperature/pressure limits, suspension handling, heating/cooling rates, robustness, and processing time.
  • Installation and testing of a 1.1 L batch microwave reactor in a kilo lab.

Main Results:

  • Successful scale-up from 15 mL to 1 L demonstrated.
  • Significant reduction in reaction times observed.
  • In some cases, improved yields and selectivity were achieved.
  • Identified limited vessel size as a major drawback for kilo-lab scale.

Conclusions:

  • Microwave technology is scalable for kilo-lab organic synthesis.
  • Current limitations in vessel size need to be addressed for broader industrial application.
  • Further development of large-scale microwave reactors is warranted.