Unity inova 500 ft nmr spectrometer

Optical rotations were determined with a JASCO P1020 digital polarimeter. IR spectra were taken on a JASCO FT/IR-4100 spectrometer. The NMR spectra were recorded on a Varian 400MR FT-NMR instrument at 400 MHz for ¹H and 100 MHz for ¹³C, and on a Varian Unity INOVA 500 FT-NMR spectrometer at 500 MHz for ¹H and 125 MHz for ¹³C in CDCl₃. LR- and HR-ESIMS were measured with a Bruker APEX II mass spectrometer. Silica gel 60 (230–400 mesh, Merck, Darmstadt, Germany) and SiliaBond C18 silica gel (40–63 µm, 60 Å, 17% carbon loading, SiliCycle, Québec, QC, Canada) were used for column chromatography. Precoated silica gel plates (Kieselgel 60 F254, Merck, Darmstadt, Germany) and precoated silica gel RP-18 plates (Kieselgel 60 F254S, Merck, Darmstadt, Germany) were used for TLC analysis.

Specific optical rotations were measured in CHCl₃ using a JASCO P-1020 digital polarimeter (JASCO Corporation, Tokyo, Japan). IR spectra were recorded on a JASCO FT/IR-4100 spectrometer and an FT/IR-4100 infrared spectrophotometer (JASCO Corporation, Tokyo, Japan). The NMR experiments were performed in CDCl₃ on a Varian 400MR FT-NMR instrument and a Varian Unity INOVA 500 FT-NMR spectrometer (Varian Inc., Palo Alto, CA, USA). LR- and HR-ESIMS were measured with a Bruker APEX II mass spectrometer and a Bruker Apex-Qe 9.4T mass spectrometer (Bruker, Bremen, Germany), respectively. Before column chromatography using Si gel or C18 gel (40–63 µm, Merck, Darmstadt, Germany), TLC analysis was performed on aluminum plates coated with Si gel or C18 gel (Kieselgel 60 F₂₅₄, 0.25 mm, Merck, Darmstadt, Germany). HPLC was performed on a Hitachi L-2455 apparatus equipped with a Supelco C18 column (ODS-3, 5 μm, 250 × 20 mm; Sciences Inc., Tokyo, Japan).