Avance 3 hd 500 ft nmr spectrometer

Optical rotations were determined on a JASCO P-2000 polarimeter (Tokyo, Japan). HR-IDA-TOF-MS were recorded on a X500 QTOF mass spectrometer (Sciex, USA). Circular dichroism (CD) spectra were acquired on a Chirascan spectrometer (Applied Photophysics, UK). The 1 H (500 MHz) and 13 C NMR (125 MHz) spectra were recorded on an AVANCE III HD 500 FT-NMR spectrometer (Bruker, Germany) with tetramethylsilane (TMS) as an internal standard. Column chromatography (CC) was performed on silica gel (Kieselgel 60, 70-230 mesh and 230-400 mesh, Merck, Darmstadt, Germany) and YMC*GEL (ODS-A, 12 nm, S-150 m, YMC Co., Ltd., Japan) resins. TLC used pre-coated silica gel 60 F 254 (Merck) and RP-18 F 254S plates (Merck), and compounds were visualised by spraying with aqueous 10% H2SO4 and heating for 3-5 min. Preparative high performance liquid chromatography (HPLC) was performed on an Agilent 1200 system (Agilent Technologies, USA) equipped with a G1361A preparative pump, a G1315D diode array detector, a G2260A preparative autosampler, and a COSMOSIL 5C 18 -MS-II Packed column (250 × 10 mm, 5 m). images taken using a Hitachi S-4800 scanning electron microscope.

Optical rotations were determined on a JASCO P-2000 polarimeter (Tokyo, Japan). UV spectra were recorded on a JASCO V-630 UV-VIS spectrophotometer (Jasco Inc., Japan). FT-IR spectra were obtained using a PerkinElmer spectrometer (L1600400 Spectrum Two DTGS, Perkin Elmer Inc., USA). HR-QTOF-MS were recorded on an Agilent 6530 Accurate-Mass spectrometer (CA, USA). The NMR spectra were recorded on a Bruker AVANCE III HD 500 FT-NMR spectrometer (Bruker, Germany) with tetramethylsilane (TMS) as an internal standard. Column chromatography (CC) was performed on silica gel (Kieselgel 60, 70-230 mesh and 230-400 mesh, Merck), YMC*Gel (ODS-A, 12 nm, S-150 mm, YMC Co., Ltd.), Sephadex ® LH-20 (25-100 μm, Merck), and Diaion ® HP-20 (250-850 µm, 260 Å, Merck) resins. TLC was used on pre-coated silica gel 60 F 254 (Merck) and RP-18 F 254S plates (Merck) and compounds were visualized by spraying with aqueous 10% H 2 SO 4 and followed by heating over 3-5 min.