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Consequently, there is a growing demand for sustainable solvents, particularly in the enzymatic synthesis and processing of polyesters. Biocatalysts offer a sustainable method for producing these materials; however, achieving high molecular weights often necessitates use of solvents. In this work, we introduce a new class of alternative aprotic solvents with medium polarity produced directly from agricultural waste biomass in up to 83\u2005mol\u2009% yield (on xylan basis). The new solvents have a largely unmodified xylose core and acetal functionality, yet they show no peroxide formation and provide reduced flammability risk. We also demonstrate their successful application in enzymatic polycondensation reactions with <jats:italic>Candida antarctica<\/jats:italic> lipase B (CaLB). In particular, the solvent dibutylxylose (DBX) outperformed the hazardous solvent diphenyl ether and facilitated polycondensation of the lignin\u2010derived diester pyridine\u20102,4\u2010dicarboxylate, yielding polyesters with a M<jats:sub>n<\/jats:sub> of &gt;15\u2005kDa. Computational modelling studies provided further insight into the molecular structure and dynamics of CaLB in the presence of new solvents. Lastly, up to 98\u2005wt\u2009% of the new xylose acetals were successfully recovered and recycled, further contributing to the sustainability of the overall process.<\/jats:p>","DOI":"10.1002\/cssc.202401877","type":"journal-article","created":{"date-parts":[[2024,10,31]],"date-time":"2024-10-31T12:40:10Z","timestamp":1730378410000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":10,"title":["Xylose Acetals \u2010 a New Class of Sustainable Solvents and Their Application in Enzymatic Polycondensation"],"prefix":"10.1002","volume":"18","author":[{"given":"Anastasia O.","family":"Komarova","sequence":"first","affiliation":[{"name":"Laboratory of Sustainable and Catalytic Processing Institute of Chemical Sciences and Engineering \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL)  Station 6 1015 Lausanne Switzerland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cicely M.","family":"Warne","sequence":"additional","affiliation":[{"name":"acib GmbH  Konrad-Lorenz-Strasse 20 3430 Tulln an der Donau Austria"},{"name":"Institute of Environmental Biotechnology Department of Agrobiotechnology IFA-Tulln University of Natural Resources and Life Sciences Vienna  Konrad-Lorenz-Strasse 20 3430 Tulln an der Donau Austria"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hugo","family":"P\u00e9tremand","sequence":"additional","affiliation":[{"name":"Laboratory of Sustainable and Catalytic Processing Institute of Chemical Sciences and Engineering \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL)  Station 6 1015 Lausanne Switzerland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Laura","family":"K\u00f6nig\u2010Mattern","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Dynamics of Complex Technical Systems Process Systems Engineering (PSE)  Sandtorstra\u00dfe 1 D-39106 Magdeburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Johannes","family":"St\u00f6ckelmaier","sequence":"additional","affiliation":[{"name":"Institute of Molecular Modeling and Simulation (MMS) University of Natural Resources and Life Sciences Vienna  Muthgasse 18 1190 Vienna Austria"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chris","family":"Oostenbrink","sequence":"additional","affiliation":[{"name":"Institute of Molecular Modeling and Simulation (MMS) University of Natural Resources and Life Sciences Vienna  Muthgasse 18 1190 Vienna Austria"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Georg M.","family":"Guebitz","sequence":"additional","affiliation":[{"name":"acib GmbH  Konrad-Lorenz-Strasse 20 3430 Tulln an der Donau Austria"},{"name":"Institute of Environmental Biotechnology Department of Agrobiotechnology IFA-Tulln University of Natural Resources and Life Sciences Vienna  Konrad-Lorenz-Strasse 20 3430 Tulln an der Donau Austria"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jeremy","family":"Luterbacher","sequence":"additional","affiliation":[{"name":"Laboratory of Sustainable and Catalytic Processing Institute of Chemical Sciences and Engineering \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL)  Station 6 1015 Lausanne Switzerland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3711-3087","authenticated-orcid":false,"given":"Alessandro","family":"Pellis","sequence":"additional","affiliation":[{"name":"Universit\u00e1 di Genova Dipartimento di Chimica e Chimica Industriale  via Dodecaneso 31 16146 Genova (GE) Italy"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2024,11,20]]},"reference":[{"key":"e_1_2_9_1_1","unstructured":"J. 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