**3. Materials and Methods**

### *3.1. General Experimental Procedures*

Optical rotation values were measured using a Jasco P-1010 digital polarimeter (Japan Spectroscopic, Tokyo, Japan). IR spectra were measured on a Thermo Scientific Nicolet iS5 FT-IR spectrophotometer (Waltham, MA, USA). NMR spectra were taken on a Jeol Resonance ECZ 400 S NMR spectrometer (Tokyo, Japan), using the residual CHCl3 signal (δ<sup>H</sup> 7.26 ppm) and CDCl3 (δ<sup>C</sup> 77.1 ppm) as the internal standard for 1H and 13C NMR, respectively; coupling constants (*J*) are presented in Hz. ESIMS and HRESIMS were recorded using a Bruker 7 Tesla solariX FTMS system. Column chromatography was carried out with silica gel (230–400 mesh, Merck, Darmstadt, Germany). TLC was performed on plates precoated with Kieselgel 60 F254 (0.25-mm-thick, Merck, Darmstadt, Germany), then sprayed with 10% H2SO4 solution followed by heating to visualize the spots. Normal-phase HPLC (NP-HPLC) was performed using a system comprised of a Hitachi L-7100 pump (Tokyo, Japan) and a Rheodyne 7725i injection port (Rohnert Park, CA, USA). Reverse-phase HPLC (RP-HPLC) was performed using a system comprised of a Hitachi L-2130 pump (Tokyo, Japan), a Hitachi L-2455 photodiode array detector (Tokyo, Japan), and a Rheodyne 7725i injection port (Rohnert Park, CA, USA). A semipreparative normal-phase column (YMC-Pack SIL, S-5 μm, 250 mm × 20 mm, Sigma-Aldrich, St. Louis, MO, USA) was used for NP-HPLC. A semipreparative reverse-phase column (Luna, 5 μm, C18(2) 100 Å, AXIA Packed, 250 mm × 21.2 mm; Phenomenex, Torrance, CA, USA) was used for RP-HPLC.
