NMR and Mass Spectrometry Protocol

Inverse detected 2D NMR spectra were measured on a ECA (500 MHz) NMR spectrometer (Jeol, Peabody, MA, USA), equipped with a 5 mm ¹H-{¹³C} probe, or an Avance III (600 MHz) NMR spectrometer (Bruker, Billerica, MA, USA), fitted with a 1.7 mm ¹H-{¹³C} microcryoprobe. High-resolution ESITOF analyses were carried out on an Agilent 1200 HPLC coupled to an Agilent 6230 TOFMS (Agilent, Santa Clara, CA, USA), calibrated immediately before measurement against an ESL-L low concentration tuning mix (part number G1969-85000, Agilent Technologies). Low-resolution MS measurements were made on a Thermoelectron Surveyor UHPLC (Thermo Fisher, Waltham, MA, USA) coupled to an MSD single-quadrupole detector. HPLC was performed on an Agilent 1200 HPLC. Other General Experimental details can be found elsewhere [50 (link)].