400 mr nmr spectrometer

Chemical shifts are reported in parts per million from TMS. All NMR spectra were recorded on an Agilent 400-MR-NMR spectrometer operated at 400 and 100 MHz for hydrogen and carbon, respectively. Data processing was carried out with the MestReNova ver.6.0.2 program. The IR spectra were obtained from a Tensor 37 FT-IR spectrometer (Bruker, Ettlingen, Germany). UV and Circular dichroism spectrums were determined on a Chirascan™ CD spectrometer. Preparative HPLC was carried out using an AGILENT 1200 HPLC system. Column chromatography (CC) was performed on silica-gel (Kieselgel 60, 70–230 mesh and 230–400 mesh, Merck, Kenilworth, NJ, USA), YMC RP-18 resins (30–50 μm, Fujisilisa Chemical Ltd., Kasugai, Aichi, Japan), or Diaion HP-20 regins (200–300 mesh, Mitsubishi Chemical Co., Chiyoda, Tokyo, Japan). For thin-layer chromatography (TLC), pre-coated silica-gel 60 F254 (0.25 mm, Merck) and RP-18 F254S (0.25 mm, Merck) plates were used.

The resonances for ¹H and ¹³C were observed at 400 and 100 MHz, respectively, in an Agilent 400-MR-NMR spectrometer. Chemical shifts are expressed in parts per million in the scale relative to tetramethylsilane. Data processing was performed by the MestReNova ver. 6.0.2 program. HR–ESI–MS analyses and prep-HPLC were carried out by an AGILENT 6550 iFunnel Q-TOF LC/MS system and by an AGILENT 1200 HPLC system, respectively. Column chromatography was done on silica–gel (Kieselgel 60, 70–230 mesh and 230–400 mesh, Merck, Kenilworth, NJ, USA) or YMC RP-18 resins (30–50 μm, Fujisilisa Chemical Ltd., Kasugai Aichi, Japan). A pre-coated silica–gel 60 F254 (0.25 mm, Merck) and RP-18 F254S plates (0.25 mm, Merck) were used for thin layer chromatography (TLC).