Table 3.
NMR dataa for 3, 4 and 5
| Position |
3b |
4c |
5e |
|||
|---|---|---|---|---|---|---|
| δH (m, J in Hz) | δC | δH (m, J in Hz) | δC | δH (m, J in Hz) | δC | |
| 2 | 2.84 (m) | 38.3 | 2.80 (t, 6.1) | 37.7 | 2.84 (d, 6.9) | 38.7 |
| 3 | 3.54 (m) | 39.9 | 3.39 (m) | 38.8 | 3.53 (m) | 39.9 |
| 4 | - | - | 8.02 (m) | - | - | - |
| 5 | - | 166.0 | - | 164.1 | - | 166.1 |
| 6 | - | 153.5 | - | 152.3 | - | 153.2 |
| 7 | 3.78 (s) | 28.5 | 3.68 (s) | 28.2 | 3.78 (s) | 28.8 |
| 8 | - | 130.8 | - | 129.3 | - | 130.7 |
| 9 | 7.36 (d, 2.0) | 134.6 | 7.28 (d, 1.8) | 133.4 | 7.35 (d, 2.0) | 134.6 |
| 10 | - | 110.6 | - | 109.5 | - | 110.6 |
| 11 | - | 153.9 | - | 153.1 | - | 153.9 |
| 12 | 6.76 (d, 8.3) | 116.9 | 6.86 (d, 8.0) | 116.9 | 6.77 (d, 8.3) | 117.2 |
| 13 | 7.06 (dd, 2.0, 8.3) | 130.2 | 6.98 (dd, 1.8, 8.0) | 129.7 | 7.05 (dd, 2.0, 8.3) | 130.5 |
| Glu | ||||||
| 1' | - | 173.1 | - | 173.0d | - | 174.4 |
| 2' | 3.52 (m) | 64.7 | 3.28 (m) | 63.0 | 3.66 (m) | 55.7 |
| N-CH3 | 2.66 (s) | 32.3 | 2.48 (s) | 32.3 | - | - |
| 3' | 2.02 (m) | 26.0 | 1.94 (m) | 26.3 | 2.14 (m) | 28.0 |
| 2.20 (m) | ||||||
| 4' | 2.55 (m) | 32.5 | 2.30 (m) | 32.6 | 2.54 (m) | 33.2 |
| 5' | - | 175.4 | - | 175.7d | - | 175.5 |
| Cys | ||||||
| N-H | - | - | 8.15 (m) | - | - | - |
| 6' | - | 173.0 | - | 171.1d | - | 172.4 |
| 7' | 4.70 (dd, 4.2, 10.0) | 54.1 | 4.24 (m) | 53.7 | 4.70 (dd, 4.5, 9.7) | 54.3 |
| 8' | 2.91 (dd, 10.0, 14.0) | 40.8 | 2.98 (m) | 42.8 | 2.93 (dd, 9.7, 14) | 41.3 |
| 3.26 (dd, 4.2, 14.0) | 3.17 (m) | 3.25 (dd, 4.5, 14) | ||||
| N-H | - | - | - | - | - | - |
| Gly | ||||||
| 9' | - | 173.4 | - | - | - | 176.2 |
| 10' | 3.82 (d, 17.0) | 42.8 | - | - | 3.77 (m) | 44.6 |
| 3.90 (d, 17.0) | ||||||
| NH4OAc | 1.93 (s) | 176.0, 22.2 | 1.95 (s) | 172.1, 19.6 | 1.95 (s) | 177.4, 22.2 |
a
Signals were assigned using a combination of gHSQC, gHMBC and gCOSY experiments.
b
CD3OD: 1H and 13C spectra were recorded at 600 and 150 MHz, respectively.
c
DMSO-d6: 1H and 13C spectra were recorded at 500 and 125 MHz, respectively.
d
These carbons were observed in a separate experiment; at 125 MHz in a Shigemi tube in DMSO-d6/CD3CN/H2O (5:2.5:1).
e
CD3OD: 1H and 13C spectra were recorded at 500 and 125 MHz, respectively.