Synthesis, structural and vibrational properties of 1-(adamantane-1-carbonyl)-3-halophenyl thioureas

Spectrochim Acta A Mol Biomol Spectrosc. 2013 Feb:102:408-13. doi: 10.1016/j.saa.2012.10.043. Epub 2012 Nov 1.

Abstract

1-(Adamantane-1-carbonyl)-3-(2,4-dichlorophenyl)thiourea (1) and 1-(adamantane-1-carbonyl)-3-(2-bromo-4,6-difluorophenyl)thiourea (2) were synthesized by the reaction of adamantane-1-carbonyl chloride with ammonium thiocyanate to afford the adamantane-1-carbonylisothiocyanate in situ followed by treatment with suitable halogenated anilines. The structures of the products were established by elemental analyses, Fourier transform infrared spectroscopy (FTIR), (1)H, (13)C nuclear magnetic resonance (NMR), mass spectroscopy and single crystal X-ray diffraction study. Bond lengths and angles show the usual values. All of three condensed cyclohexane rings of the adamantane residues adopt the usual chair conformation. The molecular conformation of 1 and 2 is stabilized by an intramolecular (NH⋯OC) hydrogen bond which forms a pseudo-six-membered ring. Structural features have been complemented with the joint analysis of the FTIR and FT-Raman spectra along with quantum chemical calculations at the B3LYP/6-311++G level.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Adamantane / analogs & derivatives*
  • Adamantane / chemical synthesis
  • Crystallography, X-Ray
  • Hydrogen Bonding
  • Magnetic Resonance Spectroscopy
  • Models, Molecular
  • Molecular Conformation
  • Quantum Theory
  • Spectroscopy, Fourier Transform Infrared
  • Spectrum Analysis, Raman
  • Thiourea / analogs & derivatives*
  • Thiourea / chemical synthesis

Substances

  • Thiourea
  • Adamantane