Lc ms 2020 system

Optical rotation data were obtained on a Rudolph Research AUTOPOL^® III automatic polarimeter. ECD data were obtained on a JASCO J-715 CD instrument. NMR data were collected on Varian 500 and 600 MHz NMR spectrometers. Intensity data were collected using a D8 Quest κ-geometry diffractometer with a Bruker Photon II cmos area detector and an Incoatec Iμs microfocus Mo Kα source (λ = 0.71073 Å). LC-MS data were obtained on a Shimadzu LC-MS 2020 system (ESI quadrupole) coupled to a photodiode array detector, with a Phenomenex Kintex 2.6 μm C₁₈ column (100 Å, 75 × 3.0 mm, 0.4 mL/min). The preparative HPLC system utilized SCL-10A VP pumps and system controller with Phenomenex Gemini 5 μm C18 column (110 Å, 250 × 21.2 mm, 10 mL/min), the analytical and semi-preparative HPLC system utilized Waters 1525 binary pumps with Waters 2998 photodiode array detectors, and Phenomenex Gemini 5 μm Gemini C₁₈, Phenomenex Kinetex 5 μm biphenyl, Phenomenex Kinetex 5 μm pentafluorophenyl (250 × 4.6 mm, 1 mL/min and 250 × 10 mm, 4 mL/min). Accurate mass data were collected on a Waters SYNAPT G2-Si mass spectrometer. All solvents were of ACS grade or better.

Optical rotation data were measured on a Rudolph Research AUTOPOL® III automatic polarimeter. NMR data were collected on Varian 400 and 500 MHz NMR spectrometers. LC-MS data were obtained on a Shimadzu LC-MS 2020 system (ESI quadrupole) coupled to a photodiode array detector, with a Phenomenex Kintex 2.6 μm C₁₈ column (100 Å, 75 × 3.0 mm, 0.4 mL/min). The preparative HPLC system utilized SCL-10A VP pumps and system controller with a Phenomenex Gemini 5 μm C₁₈ column (110 Å, 250 × 21.2 mm, 10 mL/min). Analytical and semi-preparative HPLC were performed using Waters 1525 binary pumps with Waters 2998 photodiode array detector and Phenomenex Gemini 5 μm C₁₈ and Kinetex 5 μm biphenyl (250 × 4.6 mm, 1 mL/min and 250 × 10 mm, 4 mL/min) columns. Accurate mass data were collected on an Agilent 6538 HRESI QTOF MS coupled to an Agilent 1290 HPLC and a Waters SYNAPT G2-Si mass spectrometer. Chiral analyses were performed using Waters 1525 binary pumps with Waters 2998 photodiode array detector coupled with Phenomenex Lux 5 μm cellulose-3 and cellulose-2 columns (250 × 4.6 mm, 1 mL/min). All solvents were of ACS grade or better.