Ecz 500 nmr spectrometer

Optical rotations were measured on a JASCO P-2000 polarimeter, UV/Vis data were obtained using a Beckman DU800 spectrophotometer, and IR spectra were recorded on a Nicolet 100 FT-IR spectrometer. NMR data were obtained on a JEOL ECZ 500 NMR spectrometer equipped with a 3 mm inverse probe (H3X), the 1,1-ADEQUATE experiment was performed on a Bruker AVANCE III 600 MHz NMR with a 1.7 mm dual tune TCI cryoprobe. NMR data were recorded in either DMSO-d₆ or methanol-d₄ and adjusted to the residual solvent peak (DMSO-d₆ δ_H 2.50, δ_C 39.52; methanol-d₄ δ_H 3.31, δ_C 49.00). For HPLC-MS analysis, a Thermo Finnigan Surveyor HPLC system with a Phenomenex Kinetex 5 μm C18 100 × 4.6 mm column coupled to a Thermo-Finnigan LCQ Advantage Max Mass Spectrometer was used. Samples were analyzed using a linear gradient with (A) H2O + 0.1% FA to (B) CH₃CN + 0.1% FA at a flow rate of 0.6 ml/min and UV detection at 220 nm, 254 nm and 280 nm. For HR-ESI-MS analysis, an Agilent 6530 Accurate Mass QTOF mass spectrometer was used in the positive ion mode. Semi-preparative HPLC was performed on a Thermo Fisher Scientific HPLC system with a Thermo Dionex UltiMate 3000 pump, RS autosampler, RS diode array detector, and automated fraction collector. All solvents were HPLC grade except for H₂O, which was purified by a Millipore Milli-Q system before use.