This paper describes the efficient synthesis of a [2]catenane with 87-membe
red rings and with functionalities that should enable the preparation of a
poly[2]catenane. For the ring formation, the oxidative dimerization of acet
ylenes was used. The entwinement of the rings was achieved with the help of
diphenylcarbonate as a covalent template. The structure of [2]catenane 6 w
as unambiguously proven by NMR spectroscopy. mass spectrometry, and a compa
rison of the size exclusion chromatograms of starting materials, synthetic
intermediates and products.