TABLE 3.
1H (600 MHz) and 13C (150 MHz) NMR data for compound 3 (CDCl3).
Position | δ H (J in Hz) | δ C, type | HMBC | NOESY | 1H-1H COSY |
---|---|---|---|---|---|
1 | 3.09 m | 85.1, CH | 1-OCH3 | H-3β, H-10, 1-OCH3 | H-2α, β |
2α | 2.27 m | 26.2, CH2 | — | — | H-1, H-2β, H-3α, β |
2β | 1.93 m | — | — | H-1, H-2α, H-3α, β | |
3α | 1.70 m | 35.1, CH2 | — | H-18α | H-2α, β, H-3β |
3β | 1.65 m | — | H-1, H-5 | H-2α, β, H-3α | |
4 | — | 39.3, C | — | — | — |
5 | 2.09 d (6.6) | 45.5, CH | — | H-3β, H-18α, β | H-6 |
6 | 4.10 d (6.6) | 82.3, CH | C-4, C-8, C-17, 6-OCH3 | H-9, 6-OCH3 | H-5, H-7 |
7 | 3.00 brs | 45.5, CH | C-9, C-11, C-15 | H-15, 6-OCH3 | H-6 |
8 | — | 83.7, C | — | — | — |
9 | 2.92 m | 44.4, CH | C-12, C-13, C-15 | H-6 | H-10, H-14 |
10 | 2.20 m | 42.1, CH | — | H-1, H-14 | H-9, H-12 |
11 | — | 49.9, C | — | — | — |
12α | 3.06 m | 39.3, CH2 | C-11 | — | H-10, H-12β |
12β | 1.89 m | — | H-14 | H-10, H-12α | |
13 | — | 76.2, C | — | — | — |
14 | 4.92 d (4.8) | 77.9, CH | C-8, C-16, ArC = O | H-10, H-12β | H-9 |
15 | 6.53 d (9.9) | 125.4, CH | C-9, C-13 | H-7, H-17 | H-16 |
16 | 6.05 d (9.9) | 137.3, CH | C-8 | H-17 | H-15 |
17 | 3.03 brs | 62.8, CH | C-6, C-8, C-11 | H-15, H-16, H-21, H-22 | — |
18α | 3.26 d (8.82) | 80.5, CH2 | C-3, 18-OCH3 | H-3α, H-5, H-19α, β, 18-OCH3 | H-18β |
18β | 3.65 d (8.82) | C-3, C-19, 18-OCH3 | H-5, H-19β, 18-OCH3 | H-18α | |
19α | 2.52 m | 53.8, CH2 | — | H-18α | H-19β |
19β | 2.56 m | — | H-18α, β | H-19α | |
21α | 2.50 m | 49.3, CH2 | — | H-17 | H-22 |
21β | 2.53 m | — | H-17 | H-22 | |
22 | 1.05 brs | 13.3, CH3 | — | H-17 | H-21α, β |
1-OCH3 | 3.24 s | 56.1, CH3 | C-1 | H-1 | — |
6-OCH3 | 3.15 s | 57.4, CH3 | C-6 | H-6, H-7 | — |
18-OCH3 | 3.27 s | 59.2, CH3 | C-18 | H-18α, β | — |
8-C=O | — | 169.6, C | — | — | — |
CH3 | 1.39 s | 21.8, CH3 | 8-C=O | H-2′, 6′ | — |
ArC = O | — | 166.6, C | — | — | — |
1′ | — | 122.4, C | — | — | — |
2′, 6′ | 7.94 d (6.96) | 131.7, CH | C-4′, ArC = O | 8-CO-CH3 | H-3′, 5′ |
3′, 5′ | 6.88 d (6.96) | 113.7, CH | C-1′, C-4′ | 4′-OCH3 | H-2′, 6′ |
4′ | — | 163.6, C | — | — | — |
4′-OCH3 | 3.85 s | 55.4, CH3 | C-4′ | H-3′, 5′ | — |