*3.5. Purification Procedure*

Flow chart of the isolation process of compounds **1**–**7** is presented in supporting information. Acetone extract (160 g) was impregnated with silica gel (~20 g) and loaded on an open column packed with 2 kg of silica gel. The extract was fractionated using step gradient elution using *n*-hexane, *n*-hexane: EtOAc (3:1, 1:1 and 1:3, *v*/*v*), EtOAc, EtOAc: MeOH (19:1, 9:1, 3:1, 1:1 and 1:3, *v*/*v*) to finish with MeOH. A total of 21 main fractions were pooled and dried under vacuum at 40 ◦C after analysis on silica gel TLC plates and sprayed with 10% H2SO4 in MeOH [18]. The solids from column fraction 1.11 (317.5 mg) were impregnated onto silica gel and fractionated by flash chromatography on a 40 g pre-packed cartridge and methyl *tert*-butyl ether (MTBE): acetone [(CH3)2CO] using flash chromatography. Fraction 2.4 (181 mg) was re-chromatographed using a 40 g packed RP-C18 column and ran using MeOH and MeOH: isopropanol (*i*PrOH) (9:1, *v*/*v*) to give fraction 3.3 (61 mg), which was precipitated to afford compound **1** (39 mg).

The resulting supernatant from fractions 1.11 (2.17 g) and 1.12 (11.9 g) was combined and impregnated onto silica and submitted to flash chromatography using a 120 g cartridge and a mobile gradient phase consisting of MTBE: (CH3)2CO. Fraction 4.10 (1.22 g) was submitted to similar chromatography conditions using EtOAc: (CH3)2CO. Fraction 5.5 (624 mg) was re-chromatographed on RP-C18 column (40 g) using MeOH: H2O: AcOH (92:8:0.1; *v*/*v*/%) to MeOH to furnish compound **2** (28 mg) from fraction 6.2.

The supernatant and solids from fractions 1.15 (8.7 g) and 1.16 (9 g) respectively were impregnated with silica gel and subjected to flash chromatography using a 330 g cartridge and gradient eluted with EtOAc: (CH3)2CO and (CH3)2CO: MeOH. Fraction 7.7 (8.8 g) was flash chromatographed using a RP-C18 column (40 g) with a gradient consisting of MeOH:H2O:AcOH (5:95:0.1 to 95:5:0.1 *v*/*v*/%). Fraction 8.7 (748 mg) was run in preparative HPLC using RP-C18 column and MeOH: H2O: formic acid gradient (5:95:0.1 to 95:5:0.1

*v*/*v*/%). Fraction 9.3 (55 mg) was re-chromatographed in RP-C18 preparative HPLC using ACN: H2O: formic acid (55:45: 0.1; *v*/*v*/%) to afford compound **3** (14 mg). Fractions 9.6 + 9.7 14–17 (136 mg) were subjected to RP-C18 preparative HPLC using ACN: H2O: formic acid (50:50: 0.1; *v*/*v*/%) to furnish compound **4** (13.9 mg) and compound **5** (31 mg). Fractions 8.5, 8.6, 7.4 and 7.6 were combined and ran using a 120 g RP-C18 cartridge and a MeOH: H2O: AcOH gradient. Fractions 11.8 (347 mg) and 11.10 (0.52 g) were individually re-chromatographed on RP-C18 preparative HPLC using ACN: H2O: formic acid (45:55:0.1; *v*/*v*/% and 60:40: 0.1) to give compound **6** (14.4 mg) and compound **7** (7.3 mg).
