Example 1
Unless otherwise stated, all commercially available materials were purchased from Bachem, Aldrich, P3 BioSystems, or other vendors and were used as received. All non-aqueous reactions were performed under argon in oven-dried glassware. Routine monitoring of reactions was performed using Waters Acquity Ultra Performance Liquid Chromatography (UPLC). All HPLC purifications were done by Varian PrepStar HPLC system or Waters Autopure (mass directed purification system) using Prep C18 5 μm OBD (19×150 mm) column. 1H- and 13C-NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shifts 6 are expressed in parts per million, with the solvent resonance as an internal standard (chloroform-d, 1H: 7.26; 13C: 77.16 ppm; DMSO-d6, 1H: 2.50 ppm; 13C: 39.52 ppm). Hexafluorobenzene was used as internal standard for 19F NMR. NMR data are reported as following: chemical shift, multiplicity (s=singlet, d=doublet, t=triplet, q=quartet, m=multiplet, br=broad), coupling constant, and integration.