Table 2.
5 (MeOH-d4) | 5 (DMF-d7) | ||||||
---|---|---|---|---|---|---|---|
position | δ Ca | δHb (J in Hz) | HMBCc | δ Ce | δHf (J in Hz) | HMBCc | ROESYd |
1 | 148.3 | 147.3 | |||||
2 | 120.6 | 119.4 | |||||
3 | 116.9 | 6.84 s | 1, 2, 4, 5 | 116.3 | 7.01 s | 1, 2, 4, 5 | OH-4 |
4 | 150.6 | 150.2 | |||||
OH-4 | 9.82 s | 3, 4, 5 | 3 | ||||
5 | 126.5 | 125.6 | |||||
6 | 116.5 | 6.44 s | 1, 2, 4, 5, 7 | 115.8 | 6.58 s | 1, 2, 4, 5, 7 | 7 |
7 | 30.0 | 3.32 d (7.9) | 4, 5, 6, 8, 9 | 29.3 | 3.41 d (7.5) | 1, 4, 5, 8, 9 | 6, 8, 10 |
8 | 127.6 | 5.73 t (7.9) | 5, 7, 9, 10 | 127.3 | 5.74 t (7.5) | 5, 7, 9, 10 | 7 |
9 | 134.2 | 133.2 | |||||
10 | 40.5 | 3.52 br s | 8, 9, 11, 12 | 39.7 | 3.61 br s | 8, 9, 11, 12 | 7, 12 |
11 | 140.9 | 139.8 | |||||
12, 16 | 108.1 | 6.16 br d (1.9) | 10, 13, 14, 16 | 107.2 | 6.25 br s | 10, 13, 14, 16 | OH-13 |
13, 15 | 159.3 | 159.3 | |||||
OH-13, OH-15 |
9.34 s | 12, 13, 14 | 12, 14 | ||||
14 | 101.6 | 6.13 br d (1.9) | 12, 13 | 101.2 | 6.26 d (1.8) | 12, 13 | OH-13 |
1′ | 146.8 | 146.6 | |||||
OH-1′ | 9.52 s | 1′, 2′, 6′ | 6′ | ||||
2′ | 119.1 | 120.3 | |||||
3′ | 116.8 | 6.74 s | 1′, 2′, 4′, 5′ | 115.9 | 6.91 s | 1′, 2′, 5′ | OH-4′ |
4′ | 149.4 | 148.8 | |||||
OH-4′ | 9.55 s | 3′, 4′, 5′ | 3′ | ||||
5′ | 127.1 | 126.1 | |||||
6′ | 118.4 | 6.70 s | 1′, 2′, 4′, 5′, 7′ | 117.8 | 6.90 s | 2′, 4′, 7′ | OH-1′, 7′, 8′ |
7′ | 29.9 | 3.41 d (7.9) | 4′, 5′, 6′, 8′, 9′ | 29.0 | 3.48 | 5′, 6′, 8′, 9′ | 6′, 8′, 10′ |
8′ | 128.3 | 5.88 t (7.9) | 5′, 7′, 9′, 10′ | 127.5 | 5.92 t (7.7) | 5′, 9′, 10′ | 6′, 7′ |
9′ | 133.4 | 133.1 | |||||
10′ | 40.3 | 3.69 br s | 8′, 9′, 11′, 12′ | 39.3 | 3.74 br s | 8′, 9′, 11′, 12′ | 7′, 12′ |
11′ | 136.4 | 135.1 | |||||
12′, 16′ | 109.3 | 6.41 s | 10′, 12′, 13′, 14′ | 108.3 | 6.49 | 11′, 12′, 13′, 14′ | 10′, OH-13′ |
13′, 15′ | 151.6 | 151.5 | |||||
OH-13′, OH-15′ |
9.60 s | 12′, 13′, 14′ | 12′ | ||||
14′ | 130.3 | 129.4 |
Recorded at 125 MHz; referenced to residual MeOH-d4 at δ 49.1.
Recorded at 500 MHz; referenced to residual MeOH-d4 at δ 3.30.
Proton showing HMBC correlation to indicated carbon.
Proton showing ROESY correlation to indicated carbon.
Recorded at 125 MHz; referenced to residual DMF-d7 at δ 34.89.
Recorded at 500 MHz; referenced to residual DMF-d7 at δ 2.92.