Perkin elmer 323 polarimeter

The melting points (uncorrected) were determined on a Fisher-Jhons apparatus (Fisher Scientific Company, Pittsburgh, PA, USA). The optical rotations were measured on a Perkin-Elmer 323 polarimeter (Perkin Elmer Inc., London, UK). The UV spectra were recorded on a Shimadzu UV 160U spectrophotometer (Shimadzu, Kyoto, Japan). VCD data were acquired on a BioTools dualPEM ChiralIR FT-VCD spectrophotometer (Jupiter, FL, USA). The IR spectra were obtained on a Bruker Tensor 27 spectrometer (Bruker, Ettlingen, Germany); 1D and 2D NMR experiments were performed on a Bruker Advance III HD spectrometer (Bruker Corporation, Billerica, MA, USA) at 700 MHz for ¹H and 175 MHz for ¹³C. Chemical shifts were referred to CDCl₃ (δ_H = 7.26, δ_C = 77.16). The HR-DART-MS data were acquired on a Jeol, AccuTOF JMS-T100LC mass spectrometer (Jeol Ltd., Tokyo, Japan); silica gel 230–400 mesh (Macherey-Nagel, Macherey Nagel, Düren, Germany), Sephadex LH-20 (Pharmacia Biotech AB, Uppsala, Sweden), and octadecyl-functionalized silica gel (Sigma-Aldrich, St. Louis, MO, USA) were used for column chromatography. The X-ray data were collected on an Agilent Xcalibur Atlas Gemini diffractometer (Agilent Technologies, Oxfordshire, UK).

The melting points (uncorrected) were determined on a Fisher-Johns (Fisher Scientific Company, Pittsburgh, PA, USA) apparatus. The optical rotations were measured on a Perkin-Elmer 323 polarimeter (Perkin Elmer Inc., London, UK). The ECD spectra were recorded on a Jasco J-1500 spectropolarimeter (Jasco, Tokyo, Japan) in MeOH at 1000 ppm. The IR spectra were obtained on a Bruker Tensor 27 spectrometer (Bruker, Ettlingen, Germany); 1D and 2D NMR experiments were performed on a Bruker Advance III HD spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) at 500 MHz for ¹H and 125 MHz for ¹³C and on a Bruker Advance III HD spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) at 700 MHz for ¹H and 175 MHz for ¹³C, using CDCl₃ as solvent. Chemical shifts were referred to residual CHCl₃ (δ_H = 7.26, δ_C = 77.16). The DART-MS data were obtained on a Jeol, The AccuTOF JMS-T100LC mass spectrometer. (Jeol Ltd., Tokyo, Japan) The X-ray data were collected on a Bruker D8 Venture (Bruker AXS GmbH, Karlsruhe, Germany) using CuKα (λ = 1.54178 Å). Silica gel 230-400 mesh (Macherey-Nagel, Nagel, Macherey Nagel, Düren, Germany), Sephadex LH-20 (Pharmacia Biotech AB, Uppsala, Sweden) and octadecyl-functionalized silica gel (Sigma-Aldrich, St. Louis, MO, USA) were used for column chromatography.