1H and 13C NMR dataa (δ in ppm) of 11 and 12 in C5D5N.
No. | 11 | 12 | ||
---|---|---|---|---|
δ H (J in Hz)b | δ C c | δ H (J in Hz)b | δ C c | |
1α | 1.60, m | 41.1 | 1.55, m | 41.3 |
1β | 2.70 br d (11.7) | 2.75, br d (13.2) | ||
2 | 1.69, m; 1.78, m | 23.7 | 1.74, m; 1.99, m | 24.2 |
3 | 5.75, dd (12.0, 5.6) | 78.0 | 5.82, dd (12.1, 4.5) | 78.1 |
4 | 52.4 | 52.6 | ||
5 | 2.09, br d (11.3) | 51.7 | 2.05, br d (10.0) | 51.7 |
6 | 1.60, m; 1.78, m | 21.3 | 1.58, m; 1.75, m | 21.3 |
7 | 1.27, m; 1.73, m | 33.9 | 1.25, m; 1.70, m | 34.4 |
8 | 42.8 | 41.5 | ||
9 | 2.15, d (8.8) | 52.5 | 2.10, d (10.4) | 50.8 |
10 | 38.1 | 37.8 | ||
11 | 5.36, d (8.8) | 68.1 | 4.77, d (10.4) | 67.7 |
12 | 146.6 | 145.6 | ||
13 | 113.9 | 121.6 | ||
14 | 41.0 | 43.2 | ||
15 | 0.92, m; 1.75, m | 27.3 | 0.92, m; 1.73, m | 27.2 |
16 | 0.79, m; 2.02, m | 27.9 | 0.77, m; 2.00, m | 27.8 |
17 | 33.3 | 33.6 | ||
18 | 2.68, d (10.7) | 46.0 | 2.86, d (11.1) | 46.6 |
19 | 1.50, m | 41.3 | 1.47, m | 39.8 |
20 | 0.76, m | 39.5 | 1.01, m | 39.7 |
21 | 1.25, m; 1.31, m | 31.6 | 1.28, m; 1.45, m | 31.5 |
22 | 1.28, m; 1.41, m | 41.9 | 1.29, m; 1.40, m | 41.3 |
23 | 179.2 | 179.2 | ||
24 | 1.62, s | 12.9 | 1.52, s | 12.8 |
25 | 1.45, s | 17.2 | 0.80, s | 16.2 |
26 | 1.20, s | 18.2 | 1.14, s | 18.6 |
27 | 1.34, s | 24.2 | 1.32, s | 23.9 |
28 | 0.91, s | 28.9 | 0.88, s | 28.6 |
29 | 1.32, d (6.2) | 17.1 | 1.25, d (6.5) | 18.0 |
30 | 0.88, d (6.2) | 21.0 | 0.91, d (6.4) | 21.0 |
1′ | 132.1 | 128.0 | ||
2′ | 7.37, br s | 112.0 | 7.49, br s | 115.0 |
3′ | 148.6 | 148.2 | ||
4′ | 148.2 | 148.1 | ||
5′ | 7.28, d (7.9) | 116.4 | 7.26, d (7.8) | 115.8 |
6′ | 7.23, br d (7.9) | 121.1 | 7.48, br d (7.8) | 123.5 |
7′ | 5.22, d (10.4) | 77.9 | 5.20, d (3.7) | 75.2 |
8′ | 4.99, dd (10.5, 3.1) | 77.6 | 4.88, ddd (7.1, 5.5, 3.7) | 81.2 |
9′ | 3.88, dd (11.9, 4.6) | 62.2 | 4.03, dd (12.0, 5.5) | 62.7 |
4.04, br d (11.9) | 4.29, dd (12.0, 7.1) | |||
3.86, s | 55.9 | 3.83, s | 55.9 | |
169.9 | 170.0 | |||
1.91, s | 21.3 | 1.91, s | 21.2 |
Assignments were made by a combination of 1D and 2D NMR experiments.
measured at 400 MHz.
measured at 150 MHz.