Ft 710 fourier transform infrared spectrophotometer

Optical rotations were determined on a P-1030 digital polarimeter (JASCO, Tokyo, Japan). IR spectra were measured on a FT-710 Fourier transform infrared spectrophotometer (Horiba, Kyoto, Japan), while UV spectra were taken on a V-520 UV/Vis spectrophotometer (JASCO, Tokyo, Japan). NMR data were obtained by an Ultrashield 600 spectrometer (Bruker, Ettlingen, Germany) with tetramethylsilane (TMS) as an internal standard. Positive ion HR-ESI-MS measurement was performed with the LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). Column chromatography (CC) was carried out on silica gel 60 (E. Merck, Darmstadt, Germany), and octadecyl silica (ODS) gel (Cosmosil 75C18-OPN (NacalaiTesque, Kyoto, Japan; Φ = 35 mm, L = 350 mm). HPLC was performed on ODS gel (Inertsil ODS-3, GL-science, Φ = 6 mm, 250 mm, flow rate = 1.6 mL/min, GL Sciences, Tokyo, Japan), and the eluate was observed by refractive index detector with the RI-930 intelligent detector (JASCO, Tokyo, Japan) and a PU-1580 intelligent pump (JASCO, Tokyo, Japan). All chemicals were purchased from Wako Pure Chemical Industries, Ltd. (Osaka, Japan) and TCI (Tokyo, Japan).

Optical rotations were measured on a JASCO P-1030 polarimeter (Jasco, Tokyo, Japan). UV and IR spectra were obtained on a Jasco V-520 UV/Vis spectrophotometer and a Horiba FT-710 Fourier transform infrared spectrophotometer (Horiba, Kyoto, Japan), respectively. NMR experiments were measured on a Bruker Avance 500, 600 and 700 MHz spectrometers (Bruker, Billerica, MA, USA), with tetramethylsilane (TMS) as an internal standard. Positive ion HR-ESI-MS spectra were recorded using a LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). Column chromatography (CC) was performed on Diaion HP-20 (Mitsubishi Chemical Corp., Tokyo, Japan), silica gel 60 (230–400 mesh, Merck, Darmstadt, Germany), and octadecyl silica (ODS) gel (Cosmosil 75C₁₈-OPN (Nacalai Tesque, Kyoto, Japan; Φ = 35 mm, L = 350 mm), and TLC was performed on precoated silica gel plates 60 GF₂₅₄ (0.25 mm in thickness, Merck). HPLC was performed on ODS gel (Inertsil ODS-3, GL-science, 10 mm × 250 mm, flow rate 2.5 mL/min) with a mixture of H₂O, acetone and MeOH, and the eluate was monitored by refractive index and/or a UV detector. An amino column (Shodex Asahipak NH2P-50 4E (4.6 mm × 250 mm), CH₃CN-H₂O (3:1) 1 mL/min) together with a chiral detector (Jasco OR-2090plus) was used for HPLC analysis of sugars obtained after hydrolysis [15 (link)].