Table 1. 1H NMR data for compounds 1–7 (500 MHz, J in Hz).
| no. | 1a | 2a | 3a | 4a | 5b | 6a | 7a |
|---|---|---|---|---|---|---|---|
| 1 | 2.27, dd (17.2, 8.3) | 2.27, m | 2.05, m | 1.92, m | |||
| 2α | 1.30, m | 2.28c, m | 1.98, m | 1.63, m | 2.22, m | 1.88, m | 2.00, m |
| 2β | 1.67, m | 2.61, m | 1.67, m | 1.19c, m | 2.13, m | 1.64, m | 1.34c, m |
| 3α | 1.27, m | 2.11, m | 1.66, m | 1.35c, m (2 H) | 1.32c, m (2 H) | 2.60, m | 2.82, br t (12.4) |
| 3β | 1.62, m | 1.68, m | 1.50, m | 2.22, ddd (12.3, 9.1, 1.9) | 2.23, m | ||
| 4 | 2.02, m | 1.58, m | 1.77, m | 1.70, m | |||
| 5 | 1.36c, m | 3.86, d (10.6) | |||||
| 6 | 0.61, br t | 4.46, br s | 0.40, d (9.6) | 0.62, d (9.8) | 0.59, d (9.2) | 0.90, m | 2.27, d (10.1) |
| 7 | 0.70, m | 2.29, m | 0.73, td (9.6, 3.4) | 0.95c, m | 0.79, m | 0.68, m | 1.34c, m |
| 8α | 1.87, m | 2.28c, m | 2.03, m | 1.92, m | 1.99, m | 1.75, m | 1.61, m |
| 8β | 0.99c, m | 1.31, m | 1.34, m | 1.13, m | 1.40, m | 1.63, m | 1.03, m |
| 9α | 1.63c, m | 1.88, m | 1.17, m | 1.47, m | 1.86, m | 2.09, m | 2.06, m |
| 9β | 2.21, m | 1.65, m | 1.31, m | 1.73, m | 2.62, br dd (13.8, 3.3) | 1.84, m | 1.58, m |
| 10 | 1.36, m | ||||||
| 12d | 1.02, s | 1.35, s | 1.18, s | 1.23, s | 1.04, s | 1.03, s | 1.30, s |
| 13 | 1.04, s | 1.47, s | 1.00, s | 1.04, s | 0.98, s | 1.08, s | 1.06, s |
| 14α | 1.80, m | 1.28, s | 1.15, s | 1.19c, s | 1.02, s | 1.42, s | 1.31, s |
| 14β | 2.05, m | ||||||
| 15a | 0.93, d (7.1) | 0.97, s | 1.02, d (6.7) | 0.95c, d (6.9) | 0.96, d (6.9) | 5.41, s | 5.71, s |
| 15b | 5.08, s | 5.50, s | |||||
| 7′ | 3.02, m | 3.21, dd (11.2, 2.5) | 3.29, dd (8.1, 4.7) | 2.85, m | 4.26, dd (10.1, 6.5) | 3.02, m | 3.05, m |
| 8′a | 1.63c, m | 1.84, m | 1.69, m | 2.37, m | 2.05, m | 1.48, m | 1.49, m |
| 8′b | 1.36c, m | 1.41, m | 1.52, m | 1.23, m | 1.25, m | 1.38, m | 1.34c, m |
| 9′ | 1.71, m | 1.15, m | 1.70, m | 1.67, m | 1.38, m | 1.80, m | 1.85, m |
| 10′ | 0.99c, d (6.3) | 0.88, d (6.5) | 0.96, d (5.5) | 0.97, d (6.5) | 0.86, d (6.5) | 0.99, d (6.4) | 0.97, d (6.4) |
| 11′ | 0.94, d (6.3) | 0.79, d (6.5) | 0.95, d (5.5) | 0.94, d (6.5) | 0.84, d (6.5) | 0.87, d (6.4) | 0.88, d (6.4) |
| 12′ | 10.03, s | 10.11, s | 9.84, s | 10.01, s | 9.89c, s | 9.99, s | 9.96, s |
| 13′ | 10.14, s | 10.27, s | 10.10, s | 10.12, s | 9.89c, s | 10.15, s | 10.15, s |
| OH-1′ | 13.31, s | 13.27, s | 13.04, s | 13.65, s | 13.32, s | 13.30, s | |
| OH-5′ | 13.46, s | 13.21, s | 12.81, s | 13.39, s | 13.43, s | 13.42, s |
aMeasured in CDCl3.
bMeasured in CD3OD.
cOverlapped.
dβ-oriented.