Table 1.
No. | δC, mult. b | δH (J in Hz) | COSY | HMBCc |
---|---|---|---|---|
1 | 148.8, C | |||
2 | 135.7, C | |||
3 | 126.7, C | |||
4 | 139.3, C | |||
5 | 129.1, CH | 6.64, d (8.0) | 6 | 3, 4, 6, 7, 13 |
6 | 125.3, CH | 7.08, d (8.0) | 5 | 2, 4, 5, 7, 8 |
7 | 147.7, C | |||
8 | 83.2, CH | 5.87, s | 1, 2, 6, 7, 9, 10, 21 | |
9 | 99.8, C | |||
10 | 135.5, CH | 6.62, d (5.3) | 11 | 1, 8, 9, 11, 12 |
11 | 138.0, CH | 6.65, dd (5.3, 2.1) | 10, 12 | 1, 9, 10, 12, |
12 | 129.4, CH | 6.76, d (2.1) | 11 | 1, 2, 9, 10, 11 |
13 | 73.1, CH | 4.66, dd (11.0, 4.0) | 14, 13-OH | 3, 4, 5, 14 |
14 | 65.9, CH2 | 4.23, dd (11.0, 4.0), 3.64, dd (11.0, 4.0) | 13 | 4, 13, 15 |
15 | 170.0, C | |||
16 | 42.9, CH2 | 2.57, dd (13.4, 3.8), 2.07, t (13.4) | 17 | 15, 17, 18 |
17 | 49.0, CH | 4.61, ddd (13.4, 13.4, 3.8) | 16, 17-NH | 15, 16, 18, 19, 23, 24 |
18 | 138.8, C | |||
19 | 114.2, CH | 6.52, d (2.0) | 23 | 17, 18, 20, 21, 23 |
20 | 129.2, C | |||
21 | 138.3, C | |||
22 | 151.0, C | |||
23 | 113.9, CH | 5.98, d (2.0) | 19 | 17, 18, 21, 22 |
24 | 168.4, C | |||
25 | 22.6, CH3 | 1.70, s | 24 | |
1′ | 93.1, CH | 4.45, d (8.0) | 2′ | 9, 2′, 3′, 5′ |
2′ | 69.6, CH | 2.92, dd (8.0, 3.4) | 1′, 3′ | 1′, 4′ |
3′ | 67.5, CH | 4.06, dd (8.0, 3.4) | 2′, 4′ | 1′, 5′ |
4′ | 69.6, CH | 2.98d | ||
5′ | 75.0, C | |||
4′-NMe2 | 42.9, CH3 | 2.79, br s | 4′ | |
4′-NMe2 | 44.4, CH3 | 2.79, br s | 4′ | |
6′-Meα | 31.5, CH3 | 1.43, s | 4′, 5′, 6′-Meβ | |
6′-Meβ | 20.6, CH3 | 1.46, s | 4′, 5′, 6′-Meα | |
13-OH | 5.86 | 13 | ||
17-NH | 8.41, d (8.0) | 16, 17, 24 | ||
22-OH | 8.45, s | 21, 22, 23 | ||
2′-OH | 4.95, br s | 2′ | ||
3′-OH | 5.73, br s | 3′ | ||
4′-NH+ | 9.09, br s | 4′-NMe2 |
600 MHz for 1H NMR and 150 MHz for 13C NMR.
Numbers of attached protons were determined by analysis of 2D spectra.
HMBC correlations are from the stated protons to the indicated carbons.
The coupling constant could not be determined because of overlapping signals.