Agilent 1290 uplc and autosampler

Optical rotations were recorded on a Unipol L1000 polarimeter at the sodium D-line (589.3 nm) with a 5 cm cell at 20 °C (Schmidt+Haensch, Berlin, Germany). UV and ECD were recorded on a Chirascan V100 with a 1.0 cm quartz cuvette (Applied Photophysics, Leatherhead, UK). IR data were recorded on a PerkinElmer spectrum 100 FT-IR spectrometer (PerkinElmer, Waltham, MA, USA). NMR experiments were performed on a 500 MHz Varian Inova spectrometer (Agilent, Santa Clara, CA, USA). Chemical shifts (δ in ppm) were referenced to the carbon (δ_C 39.52) and proton (δ_H 2.50) signals of DMSO-d₆. HRESIMS were obtained using an Agilent 6540 Q-Tof mass spectrometer equipped with an Agilent 1290 UPLC and autosampler (Agilent). Preparative and semipreparative HPLC was carried out on a Jasco LC-2000 series equipped with a coupled UV detector. Analytical HPLC was carried out on an Agilent 1260 HPLC system equipped with a DAD detector coupled with an Agilent 385-ELSD. All solvents used for extraction and separation were HPLC grade, and H₂O was Milli-Q (Millipore Ireland B.V., Carrigtwohill, County Cork, Ireland) filtered.

Optical rotations were
recorded at the sodium D-line (589.3 nm) on a Unipol L1000 polarimeter
with a 10 cm cell at 20 °C (Schmidt+Haensch, Berlin, Germany).
UV and ECD data were recorded in water on a Chirascan V100 with a
1.0 cm quartz cuvette (Applied Photophysics, Leatherhead, U.K.). IR
data was recorded on a PerkinElmer spectrum 100 FT-IR spectrometer
(Massachusetts, U.S.A.). NMR experiments were performed on a 500 MHz
Varian Inova spectrometer with a 5 mm OneNMR probe and a 600 MHz Agilent
Premium Compact spectrometer with a 5 mm CryoProbe (Agilent, Santa
Clara, U.S.A.). The chemical shifts (δ in ppm) are referenced
to the carbon (δ_C 49.00) and proton (δ_H 3.31) signals of residual MeOD-d₄ within the NMR solvent. High-resolution mass spectra (HRESIMS) were
obtained using an Agilent 6540 Q-Tof mass spectrometer equipped with
an Agilent 1290 UPLC and autosampler (Agilent). Large scale RP-SPE
fractionation was performed using polygoprep C₁₈-bonded
silica 35–60 μm, 120 Å (Labquip, Ireland). Semipreparative
HPLC was carried out on an Agilent 1260 HPLC system equipped with
a DAD detector. All solvents used for extraction and separations were
HPLC grade, and H₂O was milli-Q filtered. Trifluoroacetic
acid (TFA) was used for HPLC separation and was spectroscopy grade
from Alfa Aesar.