Unity as500 spectrometer

All chemical reagents were commercially available and used without further purification. Low-resolution mass spectrometry (MS) and high-resolution MS data were obtained on an Expression CMS (Advion, Ithaca, NY, USA) and a 6530 Accurate Mass quadrupole time-of-flight liquid-chromatography mass spectrometer (Agilent), respectively. Nuclear magnetic resonance (NMR) data were recorded on a Varian Unity INOVA 400 spectrometer and Varian Unity AS500 spectrometer (Agilent Technologies, Santa Clara, CA, USA) using CDCl₃, and DMSO-d₆ and chemical shifts were reported in parts per million (ppm) with reference to the respective residual solvent or deuterated peaks (δ_H 7.24 and δ_C 77.0 for CDCl₃, δ_H 2.50 and δ_C 39.7 for DMSO-d₆). Coupling constants are reported in hertz. The abbreviations used are as follows: s (singlet), d (doublet), t (triplets), q (quartet), or dd (doublet of doublets). All the reactions described below were performed under a nitrogen atmosphere and monitored by thin-layer chromatography (TLC). TLC was performed on Merck precoated 60F₂₅₄ plates. All anhydrous solvents were distilled over CaH₂ or Na/benzophenone prior to use. The identities of all final compounds was confirmed by 1D (¹H and ¹³C) and low- and high-resolution mass spectrometry.

All reagents were obtained commercially and used without further purification. Thin-layer chromatography (TLC) and column chromatography were conducted on Merck precoated 60F245 plates and MP Silica 40–63, 60 Å, respectively. High-resolution (HR) mass spectroscopy data were obtained on an Agilent Accurate Mass Q-TOF (quadruple time-of-flight) liquid chromatography (LC) mass spectrometer (Agilent, Santa Clara, CA, USA) in ESI-positive mode. Nuclear magnetic resonance (NMR) spectra were recorded on a Varian Unity INOVA 400 spectrometer or a Varian Unity AS500 spectrometer (Agilent Technologies, Santa Clara, CA, USA) for ¹H NMR (400 and 500 MHz) and for ¹³C NMR (100 MHz). DMSO-d₆, CD₃OD and CDCl₃ were used as solvents for NMR samples. The coupling constant (J) and chemical shift values were measured in hertz (Hz) and parts per million (ppm), respectively. The abbreviations used in the analysis of ¹H NMR data are follows: s (singlet), brs (broad singlet), d (doublet), dd (doublet of doublets), t (triplet), td (triplet of doublets), q (quartet) and m (multiplet).

Reagents and chemicals were obtained commercially and used without further purification. All reactions were monitored by thin layer chromatography (TLC) using Merck precoated 60F₂₄₅ plates, and reaction mixtures were purified by column chromatography using MP Silica 40–63 (60 Å). Mass spectroscopy was performed in electrospray ionization (ESI) positive mode using an Expression CMA spectrometer (Advion Ithaca, NY, USA). ¹H NMR (400 and 500 MHz) and ¹³C NMR (100 and 125 MHz) data were obtained using a Varian Unity INOVA 400 spectrometer or a Varian Unity AS500 spectrometer (Agilent Technologies, Santa Clara, CA, USA). DMSO‑d₆ and CDCl₃ were used as NMR solvents. Chemical shift values were recorded in parts per million (ppm) and coupling constants (J) were recorded in hertz (Hz). The following abbreviations are used: s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet), and brs (broad singlet).