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Zn(OAc)<jats:sub>2<\/jats:sub> offered the best performance among the salts tested. The addition of an N\u2010donor ligand such as 1,10\u2010phenanthroline increased the yield. The best catalytic performance of Zn(OAc)<jats:sub>2<\/jats:sub> can be explained by carboxylate\u2010assisted proton activation. The interaction between the substrate and the catalyst can be observed by chemical shifts in <jats:sup>1<\/jats:sup>H and <jats:sup>15<\/jats:sup>N\u2005NMR spectra. Isocyanate was a key intermediate, which was generated from amine and CO<jats:sub>2<\/jats:sub>. Silicate ester was finally converted to siloxane, which was determined by <jats:sup>29<\/jats:sup>Si\u2005NMR. The commercially available catalyst system could be reused. 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