Table 1.
1H NMR Data [δH (mult, JH)] for Compounds 1–3
| position | 1a | 2b | 3c |
|---|---|---|---|
| 1α | 1.49 (ddd, 13, 13, 2.5) | 1.39 (ddd 13, 13, 4.9) | 1.05 (m) |
| 1β | 1.26 (br d, 13) | 1.33 (m) | 1.63 (m) |
| 2 | 1.44 (m), 1.53 (m) | 1.50 (br m) | 1.59 (br m) |
| 3α | 0.95 (ddd, 13, 13, 5.7) | 1.02 (ddd, 13, 13, 5.7) | 1.28 (m) |
| 3β | 1.69 (br d, 13) | 1.66 (br d, 13) | 1.42 (dd, 12, 2.6) |
| 5 | 1.60 (dd, 11, 5.5) | 1.50 (m) | 1.05 (dd, 12, 5.5) |
| 6 | 1.95 (br m) | 1.97 (br m) | 1.29 (m), 1.70 (m) |
| 7 (or 7α) | 5.44 (br s) | 5.72 (br s) | 1.98 (ddd, 13, 13, 4.9) |
| 7β | -- | -- | 2.35 (ddd, 13, 4.0, 2.3) |
| 9 | 2.08 (br d, 13) | 2.18 (br d, 13) | 1.69 (m) |
| 11α | 0.96 (dd, 13, 5.7) | 1.10 (dd, 13, 5.7) | 2.14 (dd, 15, 11) |
| 11β | 2.35 (t, 13) | 2.35 (t, 13) | 2.25 (dd, 15, 2.3) |
| 12α | 2.54 (br d, 14) | 2.94 (br d, 15) | 4.81 (s) |
| 12β | 2.31 (d, 14) | 2.48 (d, 15) | 4.44 (s) |
| 13a | 3.02 (dd, 11, 5.6) | 3.14 (dd, 11, 6.0) | 3.08 (d, 11) |
| 13b | 3.33 (dd, 11, 5.6) | 3.36 (dd, 11, 6.0) | 3.39 (d, 11) |
| 13-OH | 3.60 (t, 5.6) | * | * |
| 14 | 0.85 (s) | 0.88 (s) | 0.71 (s) |
| 15 | 0.91 (s) | 0.90 (s) | 0.72 (s) |
| 1′-OH | 3.78 (br s) | 2.06 (s) | |
| 2′ | 3.01 (s) | 3.45 (s) | 3.63 (s) |
| 4′ | 4.38 (br d, 7.1) | -- | -- |
| 4′-OH | 3.88 (d, 7.1) | -- | -- |
| 5′ | 3.15 (d, 2.7) | 3.33 (s) | 3.82 (s) |
| 7′α | 3.45 (d, 12) | 3.88 (dd, 13, 5.7) | 3.91 (d, 14) |
| 7′β | 3.84 (d, 12) | 3.96 (dd, 13, 8.0) | 4.03 (d, 14) |
| 7′-OH | 4.31 (br s) | 1.81 (dd, 8.0, 5.7) | * |
a
Acetone-d6, 600 MHz.
b
CDCl3, 600 MHz.
c
CDCl3, 300 MHz.
*
Exchangeable signals—variable or not clearly observed.