NMR spectra were recorded on a Bruker Avance III HD 500 MHz or 250 MHz spectrometer.
The chemical-shifts (δ) reported are given in parts per million (ppm) and the coupling constants (J) are in Hertz (Hz). The spin multiplicities are reported as s = singlet, d = doublet, t = triplet, q = quartet, dd = doublet of doublet, ddd = doublet of doublet of doublet, dt = doublet of triplet, td = triplet of doublet, and m = multiplet.
uPLC-MS was performed on a Waters Acquity UPLC system coupled to a Waters Acquity PDA detector, an ELS detector and an MSD (Scan Positive: 150–850). Method (pH 3): Phenomenex Kinetix-XB C18 (2.1 x 100 mm, 1.7 μm) column. Elution with a linear gradient of Water + 0.1% Formic acid and Acetonitrile + 0.1% Formic acid at a flow rate of 0.6 mL/min. Chiral SFC analysis: Waters Thar 3100 SFC system connected to Waters 2998 PDA detector, Chiralcel OD-H 25 cm. Chiral SFC separation: Water Thar SFC system with a Waters Thar FDM pump, Waters Thar Alias autoinjector, Waters Thar fraction collector and a Waters 2998 PDA detector.