The Solid-State and Solution-State Reassigned Structures of Tagitinin A, a 3,10-Epoxy-Germacrolide from Tithonia diversifolia, and the Interconversion of 3,10-Epoxy-Germacrolide Conformational Families via a Ring-Atom Flip Mechanism

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Auteur principal: Robert Glaser
Format: Artículo científico
Langue:en
Publié: Sociedad Química de México 2005
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author Robert Glaser
author_facet Robert Glaser
contents The Solid-State and Solution-State Reassigned Structures of Tagitinin A, a 3,10-Epoxy-Germacrolide from Tithonia diversifolia, and the Interconversion of 3,10-Epoxy-Germacrolide Conformational Families via a Ring-Atom Flip Mechanism Robert Glaser Abraham García María Isabel Chávez Guillermo Delgado Multidisciplinaria (Ciencias Naturales y Exactas) tagitinin A Horeau’s rule molecular modeling conformational interconversion Tagitinin A (2), a known 3,10-epoxy-germacrolide-6,7-trans-lactone isolated from Tithoniadiversifolia, was investigated by single crystal X-ray diffraction analysis. It was found to have a1β,4α,6α,7β,8β relative configuration which differed at C(1) from the 1α-orientation originallyreported in the literature which was determined by Horeau’s Rule. Analysis of the 1H NMR spectrumof 2 shows the molecule to maintain its crystallographically observed twist-chair-boat (TCB) ninememberedring conformation in acetone-d6 solution. The twist-chair-boat/skew-chair-boat type 3conformations of saturated/unsaturated nine-membered rings within 3,10-epoxy-germacrolides canbe interconverted to the skew-chair-chair (SCC) conformation by means of a C(9) ring atom flipmechanism. As a result of this conformational change, the orientation of the C(1) atom and the C(8)-oxycarbonyl moiety are transformed from diequatorial to diaxial. The reported stereochemistry of3,10-epoxy-germacrolide lactone structures, and the DFT B3LYP/6-31g(d) modeling findings inthis work indicate that tetrahedral C(1) atoms stabilize the TCB/SCB type 3 conformations, whiletheir trigonal counterparts stabilize the SCC conformation. 2005 artículo científico 1870-249X https://www.redalyc.org/articulo.oa?id=47549219 en http://www.redalyc.org/revista.oa?id=475 Journal of the Mexican Chemical Society application/pdf Sociedad Química de México Journal of the Mexican Chemical Society (México) Num.2 Vol.49
format Artículo científico
id redalyc_47549219
institution Redalyc
language en
publishDate 2005
publisher Sociedad Química de México
spellingShingle The Solid-State and Solution-State Reassigned Structures of Tagitinin A, a 3,10-Epoxy-Germacrolide from Tithonia diversifolia, and the Interconversion of 3,10-Epoxy-Germacrolide Conformational Families via a Ring-Atom Flip Mechanism
Robert Glaser
Multidisciplinaria (Ciencias Naturales y Exactas)
tagitinin A
Horeau’s rule
molecular modeling
conformational interconversion
The Solid-State and Solution-State Reassigned Structures of Tagitinin A, a 3,10-Epoxy-Germacrolide from Tithonia diversifolia, and the Interconversion of 3,10-Epoxy-Germacrolide Conformational Families via a Ring-Atom Flip Mechanism Robert Glaser Abraham García María Isabel Chávez Guillermo Delgado Multidisciplinaria (Ciencias Naturales y Exactas) tagitinin A Horeau’s rule molecular modeling conformational interconversion Tagitinin A (2), a known 3,10-epoxy-germacrolide-6,7-trans-lactone isolated from Tithoniadiversifolia, was investigated by single crystal X-ray diffraction analysis. It was found to have a1β,4α,6α,7β,8β relative configuration which differed at C(1) from the 1α-orientation originallyreported in the literature which was determined by Horeau’s Rule. Analysis of the 1H NMR spectrumof 2 shows the molecule to maintain its crystallographically observed twist-chair-boat (TCB) ninememberedring conformation in acetone-d6 solution. The twist-chair-boat/skew-chair-boat type 3conformations of saturated/unsaturated nine-membered rings within 3,10-epoxy-germacrolides canbe interconverted to the skew-chair-chair (SCC) conformation by means of a C(9) ring atom flipmechanism. As a result of this conformational change, the orientation of the C(1) atom and the C(8)-oxycarbonyl moiety are transformed from diequatorial to diaxial. The reported stereochemistry of3,10-epoxy-germacrolide lactone structures, and the DFT B3LYP/6-31g(d) modeling findings inthis work indicate that tetrahedral C(1) atoms stabilize the TCB/SCB type 3 conformations, whiletheir trigonal counterparts stabilize the SCC conformation. 2005 artículo científico 1870-249X https://www.redalyc.org/articulo.oa?id=47549219 en http://www.redalyc.org/revista.oa?id=475 Journal of the Mexican Chemical Society application/pdf Sociedad Química de México Journal of the Mexican Chemical Society (México) Num.2 Vol.49
title The Solid-State and Solution-State Reassigned Structures of Tagitinin A, a 3,10-Epoxy-Germacrolide from Tithonia diversifolia, and the Interconversion of 3,10-Epoxy-Germacrolide Conformational Families via a Ring-Atom Flip Mechanism
topic Multidisciplinaria (Ciencias Naturales y Exactas)
tagitinin A
Horeau’s rule
molecular modeling
conformational interconversion
url https://www.redalyc.org/articulo.oa?id=47549219