Table 1.
No. | δC, mult.b | δH (J in Hz) | COSY | HMBC | |
---|---|---|---|---|---|
1 | 169.0, C | ||||
2 | 71.8, CH2 | 3.81, d (2.0) | 1, 3 | ||
3 | 59.2, CH3 | 3.37, s | 2 | ||
Hle | 4-NH | 7.43, d (8.8) | 4 | 1, 9 | |
4 | 50.4, CH | 5.50, dd (8.8, 8.8) | 4-NH, 5 | 1, 5, 6, 9 | |
5 | 75.7, CH | 3.43* | 4, 5-OH, 6 | 4, 6, 7, 8, 9 | |
5-OH | 4.79, d (7.1) | 5 | |||
6 | 29.8, CH | 1.64, m | 5, 7, 8 | 4, 5, 7, 8 | |
7 | 20.8, CH3 | 0.87, d (7.1) | 6 | 5, 6, 8 | |
8 | 16.1, CH3 | 0.83, d (7.1) | 6 | 5, 6, 7 | |
9 | 173.0, C | ||||
Pip | 13-NH | 4.50, br s | 13 | 9 | |
10 | 51.5, CH | 4.95, d (4.9) | 11 | 9, 11, 12, 14 | |
11 | 26.5, CH2 | 2.09, m, 1.63, m | 10, 12 | 10, 12, 13 | |
12 | 21.4, CH2 | 1.34, m | 11, 13 | 10, 11, 13 | |
13 | 46.7, CH2 | 2.79* | 12 | 11, 12 | |
14 | 171.0, C | ||||
Ahmppa | 15-NH | 7.59, d (8.0) | |||
15 | 53.3, CH | 4.13, dd (8.0, 8.0) | 15-NH, 16, 21 | 14, 16, 17, 21, 22 | |
16 | 38.3, CH2 | 2.79* | 15 | 15, 17, 18, 21 | |
17 | 139.9, C | ||||
18, 18′ | 129.8, CH | 7.21, dd (7.4, 1.2) | 19 | 16, 17, 19, 20 | |
19, 19′ | 128.8, CH | 7.23, dd (7.4, 7.4) | 18, 20 | 17, 18, 20 | |
20 | 126.6, CH | 7.14, dd (7.4, 1.2) | 19 | 18, 19 | |
21 | 72.4, CH | 3.44* | 15, 21-OH, 22 | 15, 22, 23, 24 | |
21-OH | 5.08, d (7.1) | 21 | |||
22 | 43.7, CH | 2.23, q (6.6) | 21, 23 | 15, 21, 23, 24 | |
23 | 15.7, CH3 | 1.05, d (6.6) | 22 | 21, 22, 24 | |
24 | 174.8, C | ||||
Auba | 25-NH | 8.10, q (10.3) | 25 | 24, 28 | |
25 | 52.8, CH | 4.38, dd (10.3, 8.1) | 25-NH, 26 | 24, 26, 28 | |
26 | 23.9, CH2 | 2.15, q (10.3), 1.93, q(10.3) | 25, 27 | 25, 27, 28 | |
27 | 42.1, CH2 | 3.71 dd (10.3, 10.3), 3.43* | 26 | 25, 26, 28, 29 | |
28 | 175.2, C | ||||
29 | 153.4, C | ||||
29- NH2 | 7.40, br s, 7.74, br s |
500 MHz for 1H NMR and 75 MHz for 13C NMR.
Numbers of attached protons were determined by analysis of DEPT spectra.
The coupling constant was not determined because of overlapping signals.