Interpretation of substituent effects on 13C and 15N NMR chemical shifts in 6-substituted purines

Phys Chem Chem Phys. 2011 Sep 21;13(35):15854-64. doi: 10.1039/c1cp20680j. Epub 2011 Aug 4.

Abstract

A range of purine derivatives modified at position 6 of the basic purine skeleton exhibit a variety of biological activities. Several derivatives are used or tested nowadays for pharmacological treatments. The present work aims to analyze the effects of substituents on the electron distribution in the purine core as reflected by NMR chemical shifts. We collected a comprehensive set of experimental NMR data for a variety of 6-substituted purines (-NH(2), -NHMe, -NMe(2), -OMe, -Me, -CCH, and -CN) and determined the molecular and crystal structures of three derivatives (-NHMe, -CCH, and -CN) by X-ray diffraction. The density-functional methods calibrated in our recent study (Phys. Chem. Chem. Phys., 2010, 12, 5126) have been employed to enable understanding of the substituent-induced changes in the NMR chemical shifts of the atoms in the purine skeleton. Analyses of the nuclear shielding using localized molecular orbitals (LMOs), specifically the natural LMOs (NLMOs) and Pipek-Mezey LMOs, were used to break down the values of the isotropic (13)C and (15)N NMR chemical shifts and the chemical shift tensors into the contributions of the individual LMOs. The experimental and calculated trends in the chemical shift of the N-3 atom correlate nicely with the Hammett constants (σ(para)) and the calculated natural charges on N-3, whereas the contributions of the LMOs to the N-1 and C-6 chemical shifts are found to be more complex.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Carbon Isotopes / analysis
  • Magnetic Resonance Spectroscopy / methods*
  • Models, Molecular
  • Purines / chemistry*
  • X-Ray Diffraction

Substances

  • Carbon Isotopes
  • Purines