Table 3.
position | δ C | δH, mult., J in Hzb | HMBC (H→C) | COSY | ROESY | |||
---|---|---|---|---|---|---|---|---|
1 | β | 72.7 | 3.825 | brs | 2α/β | 2α,19 exo | ||
2 | β | 37.8 | 2.272 | dt | 2.3, 12.7 | 2α, 1β, 3 | 19 exo, 30 | |
2 | α | 37.8 | 2.741 | dt | 12.7, 3.7 | 2β, 1β, 3 | 3 | |
3 | 84.6 | 4.366 | dd | 4.2, 11.7 | 2α/β | 29, 5, 2α | ||
4 | 41.6 | |||||||
5 | 40.1 | 2.508 | dd | 2.5, 12.6 | 6α | 6α, 7β, 3 | ||
6 | β | 20.9 | 0.901 | overlapped | 6β, 5,7β | 19 endo | ||
6 | α | 20.9 | 1.721 | overlapped | 7α, 5 | 5 | ||
7 | β | 26.4 | 1.423 | overlapped | 7α, 8 | 5, 7α | ||
7 | α | 26.4 | 2.193 | overlapped | 6α, 7β, 8 | 7b, 6α, 8 | ||
8 | 49.1 | 1.787 | dd | 4.2, 12.5 | 7α | 19 endo, 6β, 2β, 15 | ||
9 | a | |||||||
9 | a | |||||||
11 | β | 26.3 | 1.429 | overlapped | 6.0, 11.3 | 11α, 12α/β | 19 exo, 11α | |
11 | α | 26.3 | 2.814 | ddd | 14.7 | 11β, 12α/β | 28, 11b, 12α | |
12 | β | 34.1 | 1.620 | overlapped | 11α, 12α | 21, 18 | ||
12 | α | 34.1 | 1.707 | overlapped | 11α, 12β | 11α | ||
13 | 41.8 | |||||||
14 | 47.8 | |||||||
15 | 81.0 | 4.291 | d | 6.8 | 18,8 | |||
16 | 112.4 | |||||||
17 | 60.8 | 1.781 | d | 10.8 | 22α | |||
18 | Me | 19.5 | 1.246 | s | 12, 13,14, 17 | 15 | ||
19 | exo | 30.6 | 0.447 | d | 4.2 | 19 endo | 11β, 2β, 1β1 | |
19 | endo | 30.6 | 0.729 | d | 4.2 | 19 exo | 6β, 30, 8 | |
20 | 23.3 | 1.743 | m | 22α | 22β | |||
21 | Me | 19.4 | 0.952 | d | 6.5 | 20, 22,17 | 20 | 12β, 22α, 22β |
22 | β | 29.6 | 1.954 | m | 22α, 23 | 21, 17 | ||
22 | α | 29.6 | 2.675 | dt | 12.1, 1.6 | 22β, 20, 23 | 20, 21, 27 | |
23 | 73.8 | 4.598 | dt | 12.1, 1.6 | 3 | 22α/β, 24 | ||
24 | 84.1 | 3.685 | d | 6.8 | ||||
26 | Me | 30.7 | 1.406 | s | 27, 25, 24 | 24 | ||
27 | Me | 25.9 | 1.262 | s | 26, 25, 24 | 22α, 22β, 23, 24 | ||
28 | Me | 11.6 | 1.186 | s | 13, 8, 14, 15 | 11α | ||
29 | Me | 25.7 | 1.430 | s | 30, 3, 4, 5 | 3 | ||
30 | Me | 14.7 | 1.147 | s | 29, 3, 4, 5 | 19 endo, 6β, 2β | ||
1' | 107.7 | 4.874 | d | 7.3 | 3 | 2' | ||
2' | 75.0 | 4.046 | dd/t | 7.3, 8.7 | 3' | |||
3' | 78.7 | 4.123 | dd/t | 8.7 | 4' | |||
4' | 71.4 | 4.206 | m | |||||
5' | α | 67.1 | 3.561 | dd | 9.5, 11.4 | 5' β | ||
5′ | β | 67.1 | 4.228 | dd | 5.3, 11.4 |
δC could not be obtained due to insufficient signal intensity.
Coupling patterns given as line distances (first-order assumptions); for a detailed interpretation of the xylp 1H spin system, see the data for 4 in Table 1.