Cd3od

NMR spectra were recorded on a Varian Inova instrument (500 MHz) at 25 °C in CDCl₃, and CD₃OD using tetramethyl silane (TMS) as an internal standard. The NMR solvents CDCl₃ and CD₃OD were purchased from Cambridge Isotope Laboratories (Tewksbury, MA, USA). Chemical shifts (δ) were reported in parts per million (ppm) and coupling constant values (J) in Hertz (Hz) relative to CDCl₃ (1H, δ 7.26; 13C, δ 77.00) or CD₃OD (1H, δ 3.4, 4.8; 13C, δ 49.3) and tetramethyl silane. The following abbreviations were used for signal multiplicities: s = singlet; d = doublet; t = triplet; q = quartet, and m = multiplet. All other solvents were of reagent grade and were purchased from Kanto Chemical (Tokyo, Japan). ESI-MS spectra were recorded on a JEOL JMS-T100LP spectrometer (JEOL, Akishima, Japan). Melting points were measured on a Micro Melting Point Apparatus (Yanaco Co., Ltd., Kumiyama, Japan). Analytical thin-layer chromatography (TLC) was performed on 0.2 mm silica gel plates (Merck 60 F-254), (Darmstadt, Germany), developed with CHCl₃:MeOH:H₂O (65:35:10, lower phase) and sprayed with a mixture of 5% ammonium molybdate and 1% cerium (IV) sulphate in 3.6 N H₂SO₄ (Hanessian stain solution), or viewed with a handheld UV lamp (UVGL-58) at 254 nm.

Structure elucidation of purified fractions was performed through nuclear magnetic resonance (NMR) spectroscopy. All NMR spectra were recorded using a Varian Inova NMR spectrometers (¹H, 500 MHz or 400 MHz; ¹³C, 125 MHz or 100 MHz) where δ-values were referenced to respective solvent signals [CD₃OD, δ_H 3.31 ppm, δ_C 49.15 ppm; DMSO-d₆, δ_H 2.50 ppm, δ_C 39.51 ppm] (Palo Alto, CA).