Inova 400 mhz spectrometer

NMR spectra were recorded on either a Varian INOVA 400 MHz spectrometer (with 5 mm Quad-Nuclear Z-Grad Probe), or a Bruker AvanceIII HD 400 MHz (with 5mm BBFO Z-gradient Smart Probe), calibrated to CH(D)Cl₃ as an internal reference (7.26 and 77.00 ppm for ¹H and ¹³C NMR spectra, respectively). Data for ¹H NMR spectra are reported in terms of chemical shift (δ, ppm), multiplicity, coupling constant (Hz), and integration. Data for ¹³C NMR spectra are reported in terms of chemical shift (δ, ppm), with multiplicity and coupling constants in the case of C–F coupling. The following abbreviations are used to denote the multiplicities; s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet, br = broad, app = apparent, or combinations of these. LC-MS and compound purity were determined using Waters Micromass ZQ 4000, equipped with a Waters 2795 Separation Module, Waters 2996 Photodiode Array Detector, and a Waters 2424 ELSD. Separations were carried out with an XBridge BEH C18, 3.5μm, 4.6 × 20 mm column, at ambient temperature (unregulated) using a mobile phase of water-methanol containing a constant 0.10 % formic acid.