Table 1.
1H and13C NMR Spectroscopic Data for Compounds 1–5 in Methanol-d 4.
| # | 1 | 2 | 3 | 4 | 5 | |||||
|---|---|---|---|---|---|---|---|---|---|---|
| δH, mult (J in Hz)a | δC b | δH, mult (J in Hz)a | δC b | δH, mult (J in Hz)a | δC b | δH, mult (J in Hz)a | δC b | δH, mult (J in Hz)a | δC b | |
| 1 | 175.7 | 174.4 | — | 175.0 | 174.7 | |||||
| 2-OMe | 3.86 s | 65.0 | 3.82 s | 64.9 | 3.90 s | 64.8 | ||||
| 3 | 4.42 t (6.0) | 62.3 | 4.48 t (6.0) | 61.8 | 4.61 t (5.5) | 58.6 | 130.2 | 102.5 | ||
| 4 | 168.6 | 168.4 | 169.3 | 159.5 | 174.7 | |||||
| 5 | 106.6 | 107.6 | 105.6 | 105.7 | 102.0 | |||||
| 6 | 4.02 brs | 66.6 | 4.17 brs | 68.2 | 4.00 brs | 66.3 | 4.13 brs | 67.5 | 4.05 brs | 66.5 |
| 7 | 72.8 | 72.4 | 72.4 | 73.0 | 72.4 | |||||
| 8 | 4.10 br d (12.0) | 88.7 | 4.04 br d (12.0) | 88.3 | 4.15 br d (11.2) | 89.1 | 4.03 br d (12.0) | 87.6 | 4.17 br d (12.0) | 88.6 |
| 9 | 1.60 m; 1.93 m | 29.5 | 1.73 m; 1.80 m | 29.0 | 1.64 m; 1.91 m | 29.2 | 1.66 m; 1.86 m | 29.1 | 1.66 m; 1.90 m | 28.9 |
| 10 | 1.37 m; 1.60 m | 28.1 | 1.37 m; 1.58 m | 27.6 | 1.40 m; 1.64 m | 27.7 | 1.39 m; 1.57 m | 27.7 | 1.39 m; 1.58 m | 27.2 |
| 11 | 1.35 m | 32.7 | 1.33 m | 32.7 | 1.34 m | 32.3 | 1.34 m | 32.5 | 1.34 m | 32.1 |
| 12 | 1.36 m | 23.7 | 1.34 m | 23.6 | 1.35 m | 23.4 | 1.34 m | 23.4 | 1.35 m | 23.1 |
| 13 | 0.91 t (6.0) | 14.4 | 0.91 t (6.0) | 14.4 | 0.92 t (6.0) | 14.2 | 0.91 t (6.0) | 13.9 | 0.91 t (6.0) | 13.9 |
| 14 | 3.01 dd (18.0, 6.0); 3.35 dd (18.0, 6.0) | 33.6 | 3.01 dd (18.0, 6.0); 3.29 dd (18.0, 6.0) | 33.1 | 3.54 m | 52.1 | 6.31 s | 110.5 | 1.64 s | 22.9 |
| 15 | 1.31 s | 20.0 | 1.23 s | 20.0 | 1.32 s | 19.8 | 1.28 s | 18.8 | 1.32 s | 19.4 |
| 1′ | 2.90 dd (14.0, 6.0); 2.98 dd (14.0, 4.0) | 38.4 | 2.81 dd (18.0, 8.7); 2.98 dd (18.0, 5.0) | 38.3 | 3.08 m; 3.51 m | 57.4 | 3.10 m; 3.27 m | 39.8 | ||
| 2′ | 4.34 dd (6.0, 4.0) | 72.5 | 4.29 dd (8.7, 5.0) | 72.2 | 4.40, brd (8.1) | 66.9 | 4.29 brs | 72.2 | ||
| 3′ | 175.9 | 175.9 | — | 177.5 | ||||||
aSpectra recorded at 500 MHz (but 400 MHz for 4 and 5). bSpectra recorded at 125 MHz (but 100 MHz for 4 and 5). Data based on 13C, HSQC, and HMBC experiments.