Ecz 400s nmr spectrometer

NMR spectra were recorded using a Jeol ECZ 400S NMR spectrometer (400 MHz), then processed with MestReNova 14. EPR spectra in water and Glycerol/water mixtures were recorded at West Virginia University using a Bruker ELEXSYS E580 X-band spectrometer and a Magnettech L-band spectrometer (Germany). Immobilized EPR spectra in trehalose/sucrose were recorded at the University of Denver on an Bruker ELEXSYS E580 with X-band and Q-Band capabilities. HRMS data were collected using a Thermo Fisher Scientific Q Exactive Mass Spectrometer with an Electron Spray Ionization (ESI) source. HPLC analyses were performed on a Waters Alliance e2695 separations module, equipped with a 2998 PDA detector. Separations were carried out using a Waters XBridge BEH C18 4.6 mm x 50 mm, 2.5 μm column at 45°C. All solvents were purchased from Fisher Scientific. All commercially available reagents were used as received without further purification. Tetrahydrofuran was purified on an Inert Pure Solv Solvent Purification system from Innovative Technologies Inc. Chloroform – ¹³C – 99 atom % was purchased from MilliporeSigma. Glycerol (99.99%) was purchased from Acros Organics. All reactions were carried out under argon in flame-dried glassware and in deoxygenated and anhydrous solvents. Solutions of ¹³C₁-PTMTC were protected from light.