Acquity ultra performance liquid chromatography

¹H- and ¹³C- NMR spectra were acquired on a Bruker DRX-500 spectrometer. Chemical shift δ is expressed in parts per million, with the solvent resonance as an internal standard (CDCl₃, ¹H: 7.26; ¹³C: 77.16 ppm; DMSO-d6, ¹H: 2.50 ppm; ¹³C: 39.52 ppm). NMR data are reported as follows: chemical shift, multiplicity (br = broad, d = doublet, q = quartet, m = multiplet, s = singlet, t = triplet), coupling constant, and integration. All reactions in aprotic solvents were performed under argon in oven-dried glassware. Reaction progress was monitored on a Waters Acquity Ultra Performance Liquid Chromatography (UPLC/MS). All HPLC purifications were performed on a Waters Autopure (mass directed purification system) equipped with a Prep C18 5μm OBD (19 × 150 mm) column. High Resolution Mass Spectra (HRMS) of final products were collected on a PE SCIEX API 100. Unless otherwise stated, all commercially available materials were purchased from Aldrich, P3 BioSystems, Combi-Blocks or other vendors and were used as received. The purity of all final compounds were > 95% as determined on a Waters Acquity Ultra Performance Liquid Chromatography (UPLC/MS) using the following method: gradient (5–95% ACN + 0.1% formic acid in water + 0.1% formic acid over 7.5 min, followed by 95% ACN + 0.1% formic acid for 0.5 min); flow rate 0.3 mL/min, column ACQUITY UPLC^® BEH C18 1.7μM (2.1 × 50mm).