1H and 13C NMRa (δ in ppm, J in Hz) of 1–4.
No. | 1 | 2 | 3 (4) | |||
---|---|---|---|---|---|---|
δ H b | δ C c | δ H b | δ C c | δ H b | δ C c | |
1 | — | 167.8 | — | 167.8 | — | 167.4 |
3 | 6.31 d (10.6) | 75.5 | 6.29 d (10.6) | 76.8 | 6.41 d (10.7) | 75.9 |
3a | — | 148.9 | — | 148.6 | — | 147.5 |
4 | — | 116.1 | — | 115.8 | — | 115.4 |
5 | — | 160.2 | — | 160.1 | — | 160.2 |
6 | — | 119.3 | — | 119.2 | — | 119.5 |
7 | — | 157.8 | — | 157.7 | — | 157.8 |
7a | — | 109.7 | — | 109.7 | — | 109.6 |
8 | 2.60 br dd (16.6, 12.8) | 35.5 | 2.58 br dd (17.0, 12.8) | 35.8 | 2.71 br dd (17.1, 12.0) | 35.0 |
3.03 br dd (16.6, 5.0) | 3.00 br dd (17.0, 5.2) | 3.09 br dd (17.1, 4.7) | ||||
9 | 3.61 m | 42.6 | 3.64 m | 42.6 | 3.57 m | 42.4 |
10 | — | 213.5 | — | 212.0 | — | 205.8 |
11 | 2.47 dd (10.6, 2.7) | 66.7 | 2.30 dd (10.6, 1.9) | 66.7 | 4.02 d (10.7) | 73.4 |
12 | 4.26 qd (6.5, 2.7) | 70.5 | 4.44 qd (6.4, 1.9) | 67.7 | — | 201.0 |
13 | 1.45 d (6.5) | 23.1 | 1.27 d (6.4) | 22.2 | 2.34 s | 30.7 |
14 | 2.18 s | 9.0 | 2.17 s | 9.0 | 2.19 s | 9.1 |
15 | 1.15 d (6.1) | 16.3 | 1.13 d (6.3) | 16.0 | 1.14 d (6.3) | 16.6 |
7-OMe | 3.95 s | 62.3 | 3.95 s | 62.3 | 3.96 s | 62.3 |
Assignments were made by a combination of 1D and 2D NMR experiments.
Measured in acetone-d6 (600 MHz).
Measured in acetone-d6 (150 MHz).