Optical rotations were determined using a Jasco P-1020 polarimeter. UV spectra were performed using an Agilent 8453 UV−vis spectrometer. IR spectra were obtained with a Perkin-Elmer Spectrum 100 FT-IR spectrometer with ATR sampling. NMR spectra were recorded on a Varian “Unity 500” spectrometer at 500/125 MHz (1H/13C). Chemical shifts were reported in ppm using residual CD3OH (δ 3.31 ppm for 1H and 49.0 ppm for 13C) and DMSO-d6 (δ 2.50 ppm for 1H and 39.5 ppm for 13C) as an internal reference. HRESI-TOFMS was performed on an Agilent 6230 TOF LC/MS chromatograph spectrometer. (+)-ESIMS were recorded using an Agilent 1100 Series LC/MSD spectrometer. HRESI-TOFMS was performed on an Agilent 6230 TOF LC/MS chromatograph spectrometer. ESI(+) and MSe were performed on an Waters UHPLC-QTOF Acquity I-Class + Xevo G2-XS.
6230 tof lc ms chromatograph spectrometer
Manufactured by Agilent Technologies
The 6230 TOF LC/MS is a high-performance liquid chromatography time-of-flight mass spectrometer designed for accurate mass measurements and analysis. It provides precise quantification and identification of molecular compounds.
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Optical
rotations were determined using a Jasco P-1020 polarimeter. UV spectra
were recorded using an Agilent 8453 ultraviolet–visible spectrometer.
IR spectra were obtained with a PerkinElmer Spectrum 100 Fourier transform
infrared spectrometer with attenuated total reflection sampling. NMR
spectra were recorded on a Varian “Unity 500” spectrometer
and a Bruker ADVANCE 500 spectrometer at 500/125 MHz (1H/13C). Chemical shifts were reported in parts per million
using residual CD3OH (δ 3.31 ppm for 1H and 49.0 ppm for 13C) as an internal reference. HRESITOFMS
was performed on an Agilent 6230 TOF LC/MS chromatograph spectrometer.
(+)-ESIMS spectra were recorded using an Agilent 1100 Series LC/MSD
spectrometer. All ESIMS/MS measurements were recorded on a QqQ-TOF
Applied Biosystems QSTAR Elite. Chiral HPLC analyses were completed
in a Chiralpak AD-H column (5 × 150 mm, H2O + 0.04%
CF3 CO2 H/CH3 CN + 0.04% CF3CO2H gradient from 20 to 84% in 16 min, flow rate: 3 mL/min).
rotations were determined using a Jasco P-1020 polarimeter. UV spectra
were recorded using an Agilent 8453 ultraviolet–visible spectrometer.
IR spectra were obtained with a PerkinElmer Spectrum 100 Fourier transform
infrared spectrometer with attenuated total reflection sampling. NMR
spectra were recorded on a Varian “Unity 500” spectrometer
and a Bruker ADVANCE 500 spectrometer at 500/125 MHz (1H/13C). Chemical shifts were reported in parts per million
using residual CD3OH (δ 3.31 ppm for 1H and 49.0 ppm for 13C) as an internal reference. HRESITOFMS
was performed on an Agilent 6230 TOF LC/MS chromatograph spectrometer.
(+)-ESIMS spectra were recorded using an Agilent 1100 Series LC/MSD
spectrometer. All ESIMS/MS measurements were recorded on a QqQ-TOF
Applied Biosystems QSTAR Elite. Chiral HPLC analyses were completed
in a Chiralpak AD-H column (5 × 150 mm, H2O + 0.04%
CF3 CO2 H/CH3 CN + 0.04% CF3CO2H gradient from 20 to 84% in 16 min, flow rate: 3 mL/min).
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