*3.1. General*

Melting points were recorded on a capillary melting point apparatus and are uncorrected. Unless otherwise specified, 1H and 13C-NMR spectra were recorded at 30 ◦C in DMSO-*d*<sup>6</sup> on a Varian INOVA 500 or 600 NMR spectrometer. The 1H- and 13C-NMR chemical shifts were referenced to the solvent peak for DMSO-*d*<sup>6</sup> at δ<sup>H</sup> 2.50 and δ<sup>C</sup> 39.5. LRESIMS was obtained from LC-MS data generated using a Waters Alliance 2790 HPLC equipped with a Waters 996 photodiode array detector and an Alltech evaporative light scattering detector that was attached to a Water ZQ mass spectrometer. HRESIMS were recorded on a Bruker (Billerica, MA, USA) MicrOTof-Q spectrometer (Dionex UltiMate 3000 micro LC system, ESI mode). Analytical thin layer chromatography (TLC) was performed on aluminum-backed 0.2 mm thick silica gel 60 F254 plates as supplied by Merck (Frankfurt, Germany). Eluted plates were visualized using a 254 nm UV lamp and/or by treatment with a suitable dip followed by heating. These dips included phosphomolybdic acid:Ce(SO4)2:H2SO4 (conc.):H2O (37.5 g:7.5 g:37.5 g:720 mL) or KMnO4:K2CO3:5% NaOH aqueous solution:H2O (3 g:20 g:5 mL:300 mL). Flash chromatographic separations were carried out following protocols defined by Still *et al*., [11] with silica gel 60 (40–63 mm, supplied by GRACE, Baulkham Hills, NSW, Australia) or amino bonded silica gel (Davisil®) as the stationary phase and using the AR- or HPLC-grade solvents indicated. Semi-preparative HPLC work was performed using a Waters 600 pump and 966 PDA detector, a Gilson 715 liquid handler and a C18-bonded silica Betasil 5 μm 143 Å column (21.2 mm × 150 mm). Alltech sample preparative C18-bonded silica (35–75 μm, 150 Å) and an Alltech stainless steel guard cartridge (10 mm × 30 mm) were used for pre-adsorption and HPLC work. A Phenomenex C18-bonded silica Luna 3 μm 100 Å (4.6 mm × 50 mm) column was used for LC-MS studies. All compounds were analyzed for purity using LC-MS and shown to be >95% pure, unless otherwise stated. Starting materials and reagents were available from the Sigma-Aldrich (St. Louis, MO, USA), Merck (Frankfurt, Germany), AK Scientific Inc. (Union City, CA, USA), Matrix Scientific Chemical (Columbia, SC, USA) and were used as supplied. MeOH and CH2Cl2 were dried using a glass contour solvent purification system that is based upon a technology originally described by Grubbs *et al*. [12]. Where necessary, reactions were performed under a nitrogen atmosphere and glassware was heated in an oven at 140 ◦C then dried under vacuum prior to use. Compounds for biological studies were placed under high vacuum (0.05 mmHg) for several hours before testing to remove trace, residual solvents.
