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Here, we disclose the alternating copolymerization of cyclic acetals (made from formaldehyde and diols) and anhydrides for the first time, using 5 cyclic acetals and 9 anhydrides to afford 45 unprecedented polyesters. At a wide range of reaction temperatures (25 to 140\u2009\u00b0C), diverse metal\u2010free Lewis\/Br\u00f8nsted acids are highly active catalysts for these copolymerizations via the cationic mechanism. Of interest, kinetic studies indicate that the copolymerization of cyclic acetals and anhydrides shifts the chemical equilibrium of \u201ccyclic acetals \u21cc polyacetals\u201d to the left, thus yielding polyesters with up to &gt;99\u2009% alternating degree. The obtained polyesters possess high oxygen content ([O]\u2009:\u2009[C] up to 6\u2009:\u20097), molecular weights of 2.0\u201333.3\u2005kDa, narrow polydispersities of 1.2\u20131.5, low glass transition temperatures (\u221264 to \u221227\u2009\u00b0C), as well as high decomposition temperatures (275 to 324\u2009\u00b0C).<\/jats:p>","DOI":"10.1002\/anie.202117316","type":"journal-article","created":{"date-parts":[[2022,1,18]],"date-time":"2022-01-18T09:52:03Z","timestamp":1642499523000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":32,"title":["A Facile and Unprecedented Route to a Library of Thermostable Formaldehyde\u2010Derived Polyesters: Highly Active and Selective Copolymerization of Cyclic Acetals and Anhydrides"],"prefix":"10.1002","volume":"61","author":[{"given":"Xun","family":"Zhang","sequence":"first","affiliation":[{"name":"MOE Key Laboratory of Macromolecular Synthesis and Functionalization International Research Center for X Polymers Department of Polymer Science and Engineering Zhejiang University Hangzhou 310027 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chengjian","family":"Zhang","sequence":"additional","affiliation":[{"name":"MOE Key Laboratory of Macromolecular Synthesis and Functionalization International Research Center for X Polymers Department of Polymer Science and Engineering Zhejiang University Hangzhou 310027 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6543-0042","authenticated-orcid":false,"given":"Xinghong","family":"Zhang","sequence":"additional","affiliation":[{"name":"MOE Key Laboratory of Macromolecular Synthesis and Functionalization International Research Center for X Polymers Department of Polymer Science and Engineering Zhejiang University Hangzhou 310027 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2022,2,7]]},"reference":[{"key":"e_1_2_3_1_1","doi-asserted-by":"publisher","DOI":"10.1021\/ar500121d"},{"key":"e_1_2_3_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.7b00209"},{"key":"e_1_2_3_3_1","doi-asserted-by":"publisher","DOI":"10.1038\/nature21001"},{"key":"e_1_2_3_4_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.297.5582.803"},{"key":"e_1_2_3_5_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.7b00329"},{"key":"e_1_2_3_6_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41578-021-00363-3"},{"key":"e_1_2_3_7_1","doi-asserted-by":"publisher","DOI":"10.1002\/adhm.201900312"},{"key":"e_1_2_3_8_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja063092m"},{"key":"e_1_2_3_9_1","doi-asserted-by":"publisher","DOI":"10.1039\/c2cs15327k"},{"key":"e_1_2_3_10_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202006807"},{"key":"e_1_2_3_10_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.202006807"},{"key":"e_1_2_3_11_1","doi-asserted-by":"publisher","DOI":"10.1021\/ma1013463"},{"key":"e_1_2_3_12_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.mattod.2021.07.024"},{"key":"e_1_2_3_13_1","doi-asserted-by":"publisher","DOI":"10.1038\/nchem.2391"},{"key":"e_1_2_3_14_1","doi-asserted-by":"publisher","DOI":"10.1038\/nchem.2574"},{"key":"e_1_2_3_15_1","doi-asserted-by":"publisher","DOI":"10.1021\/mz3005956"},{"key":"e_1_2_3_16_1","doi-asserted-by":"publisher","DOI":"10.31635\/ccschem.020.201900119"},{"key":"e_1_2_3_17_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.8b09739"},{"key":"e_1_2_3_18_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201707122"},{"key":"e_1_2_3_18_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201707122"},{"key":"e_1_2_3_19_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202104495"},{"key":"e_1_2_3_19_2","doi-asserted-by":"crossref","DOI":"10.1002\/ange.202104495","volume":"134","year":"2022","journal-title":"Angew. 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