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The impact of Novel Process Windows on the Claisen rearrangement

Tetrahedron, ISSN: 0040-4020, Vol: 69, Issue: 14, Page: 2885-2890
2013
  • 34
    Citations
  • 0
    Usage
  • 27
    Captures
  • 0
    Mentions
  • 0
    Social Media
Metric Options:   Counts1 Year3 Year

Metrics Details

  • Citations
    34
    • Citation Indexes
      34
  • Captures
    27

Article Description

The impact of Novel Process Windows on the Claisen rearrangement in microflow was investigated. Elevated temperatures (up to 300 °C) were crucial to achieve full conversion of allyl phenyl ether in the Claisen rearrangement. We observed that 1-butanol was the optimal reaction solvent for this transformation in flow. Solvent-free reaction conditions were feasible for the Claisen rearrangement and provided quantitative yields of the target product at 280 °C and 100 bar. Also elevated reaction pressures (up to 300 bar) were investigated in the Claisen rearrangement. We found that thermal expansion and pressure-related compression phenomena cannot be ignored at such harsh reaction conditions. These phenomena lead to large deviations of the desired residence time (as calculated from the nominal flow rate) and have a clear impact on the observed reaction trends. Finally, we also investigated the temperature effect on the Johnson–Claisen rearrangement of cinnamyl alcohol. Quantitative yields were obtained at 200 °C and at 100 bar.

Bibliographic Details

Hiroki Kobayashi; Brian Driessen; Dannie J.G.P. van Osch; Ali Talla; Shinichi Ookawara; Timothy Noël; Volker Hessel

Elsevier BV

Biochemistry, Genetics and Molecular Biology; Pharmacology, Toxicology and Pharmaceutics; Chemistry

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