Qtof mass detector

Tetrahydrofuran was distilled from sodium benzophenone. All other solvents and chemical reagents were obtained from commercial sources and used directly without further purification. Glassware was oven-dried before use. All reactions were performed under an argon atmosphere. TLC was performed on silica gel 60 GF254 and monitored under UV light or visualized using phosphomolybdic acid reagent. Flash chromatography was performed on 230–400 mesh silica gel (Fisher Scientific). Melting points were recorded on an MPA100 Automated Melting Point Apparatus. NMR spectra were obtained on a Bruker Ascend 400 (Billerica, MA) spectrometer or a Varian Inova-500 spectrometer (Agilent Technologies, Santa Clara, CA). HR-MS were obtained on Waters Acquity UPLC linked to a Waters Acquity Photodiode Array Detector and Waters qTof mass detector. All compounds reported herein with biological data had purities ≥95% as determined by HPLC. The purity of associated compounds was verified by the HPLC study performed on BEH C18 (2.1 × 50 mm, 1.7 μm) column using a mixture of solvent acetonitrile/water (with 0.1% formic acid) at a flow rate of 0.3 mL/min and monitoring by UV absorption at the appropriate wavelength. Chemical shifts are given in ppm with tetramethylsilane (TMS) as an internal reference. All coupling constants (J) are given in hertz (Hz).

All solvents and chemical reagents were purchased from commercial sources and used directly without further purification. Glassware was oven-dried before use. All reactions were performed under an argon atmosphere. Analytical thin-layer chromatography was performed on silica gel 60 GF254 and monitored under UV light. Flash chromatography was performed on 230–400 mesh silica gel (Fisher Scientific). NMR spectra were obtained on a Bruker Ascend 400 (Billerica, MA) spectrometer. The purity of all final compounds (as stereoisomers not separable on the UPLC column used) was ≥95% as determined by UPLC and further confirmed by proton NMR (details given in the Supporting Information). High-resolution mass spectrometry data (HRMS) were obtained on a Waters Acquity UPLC linked to a Waters Acquity Photodiode Array Detector and a Waters qTof mass detector. UPLC analyses were performed using a BEH C18 (2.1 × 50 mm, 1.7 μm) column and a mixture of solvent methanol/water at a flow rate of 0.3 mL/min, monitored by UV absorption at the appropriate wavelength. Chemical shifts are given in ppm. Tetramethylsilane is used as an internal reference for NMR spectra taken in chloroform-d. All coupling constants (J) are given in hertz (Hz).