Herein, we report the efficient intramolecular dehydrative coupling of symmetrical and unsymmetrical diols for the synthesis of macrocyclic crown ethers in the presence of Ni-zeolite as a catalyst under continuous flow module. This method is also efficient for the intramolecular dehydrative macrolactonization of seco-acids using Ni-zeolite or Ru-zeolite. This flow catalysis is demonstrated by a wide substrate scope with one-time packed Ni-zeolite to produce 20 macrocyclic polyethers and 11 examples of broad macrolactones with water as a byproduct.

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http://dx.doi.org/10.1021/acs.joc.4c01692DOI Listing

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