Fraction B (1.83 g) was further
isolated by QCC with 5% EtOAc−hexanes to give four subfractions
(B1−B4). Subfraction B2 (281.4 g) was separated by repeated CC
using 30% CH2Cl2−hexanes to yield compound 7 (17.1 mg), whereas
compounds 6 (17.0 mg), 8 (3.8 mg), 16 (2.1 mg), and 18 (2.1 mg)
were derived from subfraction B4 (176.8 mg) by repeated CC with
50% CH2Cl2−hexanes. Fraction C (2.01 g) was further separated by
QCC with 10% EtOAc−hexanes to 20% EtOAc−hexanes to afford five
subfractions (C1−C5). Subfraction C2 (285.4 mg) was subjected to
CC with 20% EtOAc−hexanes to give seven fractions (C2a−C2g).
Fractions C2b (30.2 mg) and C2d (34.3 mg) were repeatedly purified
by CC using 20% CH2Cl2−hexanes, yielding compounds 1 (5.8 mg)
and 10 (16.6 mg), respectively, while compound 20 (2.8 mg) was
isolated from fraction C2f (27.6 mg) by CC with 45% CH2Cl2−
hexanes. Fraction C4 (181.9 mg) was subjected to repeated CC using
20% EtOAc−hexanes to give five subfractions (C4a−C4d). Subfractions
C4b (55.4 mg) and C4d (24.6 mg) were further purified by
CC with 80% CH2Cl2−hexanes to give compounds 17 (3.7 mg) and
15 (6.5 mg), respectively. Fraction D (3.21 g) was subjected to QCC
and eluted with increasing polarity of the elution solvent system of
hexanes and EtOAc (20% EtOAc−hexanes to 100% EtOAc) to
provide seven subfractions (D1−D7). Subfraction D2 (118.9 mg) was
further isolated by CC with 30% EtOAc−hexanes to yield compound
11 (12.8 mg). Fractions D3 (1.18 g) and D5 (862.0 mg) were
subjected to Sephadex LH-20 using MeOH to afford four (D3a−D3d)
and five (D5a−D5e) subfractions, respectively. Subfraction D3b
(751.0 mg) was separated by CC with 2% EtOAc−CH2Cl2 to yield
compound 9 (3.0 mg) and six subfractions (D3b1−D3b6).
Subfractions D3b2 (25.1 mg) and D3b4 (30.5 mg) were further
separated by CC with 25% EtOAc−hexanes to give compounds 5 (9.5
mg) and 14 (2.1 mg), respectively, while compound 19 (3.0 mg) was
derived from subfraction D3d (114.2 mg) by repeated CC with 20%
EtOAc−hexanes. Fraction D5b (259.1 mg) was further isolated by CC
with 5% EtOAc−CH2Cl2 to afford compounds 2 (2.1 mg), 12 (19.0
mg), and 13 (8.5 mg). Finally, compounds 3 (1.7 mg) and 4 (6.2
Fraction B (1.83 g) was furtherisolated by QCC with 5% EtOAc−hexanes to give four subfractions(B1−B4). Subfraction B2 (281.4 g) was separated by repeated CCusing 30% CH2Cl2−hexanes to yield compound 7 (17.1 mg), whereascompounds 6 (17.0 mg), 8 (3.8 mg), 16 (2.1 mg), and 18 (2.1 mg)were derived from subfraction B4 (176.8 mg) by repeated CC with50% CH2Cl2−hexanes. Fraction C (2.01 g) was further separated byQCC with 10% EtOAc−hexanes to 20% EtOAc−hexanes to afford fivesubfractions (C1−C5). Subfraction C2 (285.4 mg) was subjected toCC with 20% EtOAc−hexanes to give seven fractions (C2a−C2g).Fractions C2b (30.2 mg) and C2d (34.3 mg) were repeatedly purifiedby CC using 20% CH2Cl2−hexanes, yielding compounds 1 (5.8 mg)and 10 (16.6 mg), respectively, while compound 20 (2.8 mg) wasisolated from fraction C2f (27.6 mg) by CC with 45% CH2Cl2−hexanes. Fraction C4 (181.9 mg) was subjected to repeated CC using20% EtOAc−hexanes to give five subfractions (C4a−C4d). SubfractionsC4b (55.4 mg) and C4d (24.6 mg) were further purified byCC with 80% CH2Cl2−hexanes to give compounds 17 (3.7 mg) and15 (6.5 mg), respectively. Fraction D (3.21 g) was subjected to QCCand eluted with increasing polarity of the elution solvent system ofhexanes and EtOAc (20% EtOAc−hexanes to 100% EtOAc) toprovide seven subfractions (D1−D7). Subfraction D2 (118.9 mg) wasfurther isolated by CC with 30% EtOAc−hexanes to yield compound11 (12.8 mg). Fractions D3 (1.18 g) and D5 (862.0 mg) weresubjected to Sephadex LH-20 using MeOH to afford four (D3a−D3d)and five (D5a−D5e) subfractions, respectively. Subfraction D3b(751.0 mg) was separated by CC with 2% EtOAc−CH2Cl2 to yieldcompound 9 (3.0 mg) and six subfractions (D3b1−D3b6).Subfractions D3b2 (25.1 mg) and D3b4 (30.5 mg) were furtherseparated by CC with 25% EtOAc−hexanes to give compounds 5 (9.5mg) and 14 (2.1 mg), respectively, while compound 19 (3.0 mg) wasderived from subfraction D3d (114.2 mg) by repeated CC with 20%EtOAc−hexanes. Fraction D5b (259.1 mg) was further isolated by CCwith 5% EtOAc−CH2Cl2 to afford compounds 2 (2.1 mg), 12 (19.0mg), and 13 (8.5 mg). Finally, compounds 3 (1.7 mg) and 4 (6.2
การแปล กรุณารอสักครู่..