Free-Radical Epimerization of D- into L-C-(glycosyl)methanol Compounds Using 1,5-Hydrogen Atom Transfer Reaction

A simple epimerization of C-(α-D-Gly p )methanol into C-(β-L-Gly p )methanol compounds is described. The radical sequence involved homolytic cleavage of the C5–H bond by 1,5-hydrogen atom transfer promoted by the 1’-O-yl radical and subsequent hydride addition with inversion of configuration. This m...

Descripción completa

Detalles Bibliográficos
Autores: Montes, Adrián S., León, Elisa I., Martín, Ángeles, Pérez-Martín, Inés, Suárez, Ernesto
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2022
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/258275
Acceso en línea:http://hdl.handle.net/10261/258275
Access Level:acceso abierto
Palabra clave:C-Glycosides
C-H activation
Hydrogen transfer
Radical reactions
Regioselectivity
Descripción
Sumario:A simple epimerization of C-(α-D-Gly p )methanol into C-(β-L-Gly p )methanol compounds is described. The radical sequence involved homolytic cleavage of the C5–H bond by 1,5-hydrogen atom transfer promoted by the 1’-O-yl radical and subsequent hydride addition with inversion of configuration. This methodology allows the preparation of rare C-(β-L-Ido p )-, C-(β-L-Altp)-, C-(β-L-Gulp)-, C-(β-L-Allp)methanol glycosides starting from carbohydrates of the D-series. It can also be applied to transform L- into D-configured C-glycosyl compounds, as illustrated by the formation of C-(β-D-6dGulp)- and C-(β-D-6dAltp)methanol from readily accessible L-rhamno and L-fuco analogs, respectively. In further development of this procedure compounds with C-(β-L-Araf)- and C-(β-L-5dRibf)methanol structures have also been synthesized. The alkoxyl radicals were generated by reaction of the corresponding N-alkoxyphthalimides with nBu3SnH(D) and in comparative terms, by visible light-photocatalysis using the Hantzsch ester/fac-Ir(ppy)3 procedure. The influence of the sugar ring conformation and the electronegativity of the substituents on the stereochemical outcome will be addressed.