Finnigan ltq fticr ms instrument

NMR spectra were collected on a Varian Unity 500 MHz (500 MHz and 125 MHz for the ¹H and ¹³C nuclei respectively), a Varian VX 500 MHz with ¹³C-optimized cryoprobe, and a Bruker 600 MHz (600 MHz and 150 MHz for the ¹H and ¹³C nuclei respectively) with 1.7 mm inverse cryo-probe. NMR experiments were conducted using CDCl₃ from Cambridge Isotope Laboratories, Inc. 99.8% D, containing 0.03% or 1.0% v/v trimethylsilane (referencing δ_H 0.0 as the internal standard from trimethylsilane, and δ_C 0.0 or δ_C 77.16 as internal standards using trimethylsilane and CDCl₃, respectively). Microwave-heated reactions were run in a Biotage Initiator microwave synthesizer. LR-LCMS data were collected on a Thermo Finnigan Surveyor Autosampler/LC-Pump-Plus/PDA-Puls with a Thermo Finnigan Advantage Max mass spectrometer. HRMS data was collected on a Finnigan LTQ-FTICR-MS instrument (Thermo-Electron Corporation, San Jose, CA) fitted with either an Ion-Max ESI source for LCMS runs, or a Biversa Nanomate (Advion Biosystems, Ithaca, NY) electrospray source. HPLC purification was carried out with a Waters 515 HPLC Pump with a Waters 996 Photodiode Array Detector using Empower Pro software. All solvents were HPLC grade except for H₂O which was purified with a Millipore Milli-Q system before use, CH₃CN which was LCMS grade from J.T. Baker, and acetone which was distilled before use.