Star mesogens - Synthesis and structural characterization using 1D and 2D solution NMR techniques and mesophase characterization

Novel star mesogens based on trimesic acid and symmetrical side arm cores with terminal alkoxy groups were synthesized via a divergent approach. The central core and side arms were connected through alkyl spacers. All the synthesized mesogens and their intermediates were characterized thoroughly using Fourier transform infrared (FT-IR), H-1 nuclear magnetic resonance (NMR), C-13 NMR, and mass spectrometers. One representative mesogen was subjected to the two-dimensional (2D) NMR experiments to ascertain the structure of the mesogens. The mesophase characterization was carried out using hot-stage optical polarizing microscopy (HOPM), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques. Many of the molecules with an ethyloxy spacer were found to be nonmesogenic, whereas all the molecules with a butyloxy spacer showed liquid crystalline phases. The increase of terminal chain length decreased the transition temperatures. The nematic phase was observed for the mesogens with short terminal chain length, whereas smectic polymorphism was observed on increasing the terminal chain length. The results of a variable temperature powder X-ray diffraction of the representative sample support the smectic layer ordering.