Reaction Mechanism in Crystalline Solids: Kinetics and Conformational Dynamics of the Norrish Type II Biradicals from α- Adamantyl-p-Methoxyacetophenone.

In an effort to determine the details of the solid-state reaction mechanism and diastereoselectivity in the Norrish type II and Yang cyclization of crystalline α-adamantyl-p-methoxyacetophenone, we determined its solid-state quantum yields and transient kinetics using nanocrystalline suspensions. Th...

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Publicado en:Journal of the American Chemical Society Vol. 134; no. 2; pp. 1115 - 1124
Autores principales: Kuzmanich, Gregory, Vogelsberg, Cortnie S., Maverick, Emily F., Netto-Ferreira, José Carlos, Scaiano, J. C., Garcia-Garibay, Miguel A.
Formato: Artículo
Publicado: American Chemical Society 1/18/2012
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Acceso en línea:Ver este registro en EBSCOhost
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        atl: Reaction Mechanism in Crystalline Solids: Kinetics and Conformational Dynamics of the Norrish Type II Biradicals from α- Adamantyl-p-Methoxyacetophenone.
      aug:
        au:
          Kuzmanich, Gregory
          Vogelsberg, Cortnie S.
          Maverick, Emily F.
          Netto-Ferreira, José Carlos
          Scaiano, J. C.
          Garcia-Garibay, Miguel A.
        affil:
          Department of Chemistry and Biochemistry, University of California, Los Angeles, California 90095-1559, United States
          Department of Chemistry and Centre for Catalysis Research and Innovation, University of Ottawa, Ottawa, Ontario, Canada K1N 6N5
      su:
        Crystallography
        Nuclear magnetic resonance spectroscopy
        Hydrogen
        Optical diffraction
        Relaxation (Nuclear physics)
        Spin-lattice relaxation
      sug:
        subj:
          Crystallography
          Nuclear magnetic resonance spectroscopy
          Hydrogen
          Optical diffraction
          Relaxation (Nuclear physics)
          Spin-lattice relaxation
      ab: In an effort to determine the details of the solid-state reaction mechanism and diastereoselectivity in the Norrish type II and Yang cyclization of crystalline α-adamantyl-p-methoxyacetophenone, we determined its solid-state quantum yields and transient kinetics using nanocrystalline suspensions. The transient spectroscopy measurements were complemented with solid-state NMR spectroscopy spin-lattice relaxation experiments using isotopically labeled samples and with the analysis of variable-temperature anisotropic displacement parameters from single-crystal X-ray diffraction to determine the rate of interconversion of biradical conformers by rotation of the globular adamantyl group. Our experimental findings include a solid-state quantum yield for reaction that is 3 times greater than that in solution, a Norrish type II hydrogen-transfer reaction that is about 8 times faster in crystals than in solution, and a biradical decay that occurs on the same time scale as conformational exchange, which helps to explain the diastereoselectivity observed in the solid state.
      pubtype: Academic Journal
      doctype: Article
      src: R
    language: English
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