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As exampled by thymidine and adenosine, this approach involves the installation of an activating reagent, 1,3\u2010benzodithiol\u20102\u2010ylium tetrafluoroborate (BDTF), at the 3'\u2010hydroxy group of thymidine and 2'\u2010hydroxy group of adenosine under mild conditions. Subsequent visible light promoted single\u2010electron oxidation and \u03b2\u2010scission generates the key radical intermediate and afford functionalized nucleosides by reaction with a broad range of radical acceptors. This method has the advantages of excellent yields and high diastereoselectivity, offering a versatile platform for the synthesis of complex, drug\u2010relevant nucleoside derivatives. \u00a9 2026 Wiley Periodicals LLC.<\/jats:p>\n                  <jats:p>\n                    <jats:bold>Basic Protocol 1<\/jats:bold>\n                    : Synthesis of 3'\u2010\n                    <jats:italic>O\u2010<\/jats:italic>\n                    BDT\u2010thymidine and 2'\u2010\n                    <jats:italic>O\u2010<\/jats:italic>\n                    BDT\u2010adenosine\n                  <\/jats:p>\n                  <jats:p>\n                    <jats:bold>Basic Protocol 2<\/jats:bold>\n                    : Deoxygenative functionalization of 3'\u2010\n                    <jats:italic>O\u2010<\/jats:italic>\n                    BDT\u2010thymidine and 2'\u2010\n                    <jats:italic>O\u2010<\/jats:italic>\n                    BDT\u2010adenosine\n                  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