TABLE 3.
Assignment of NMR signalsa of glycan on S201 of the D200-A211 peptide
| Residuea | Position |
1H NMR
|
13C NMR δ (ppm) | ||
|---|---|---|---|---|---|
| δ (ppm) | Multiplicityb (W1/2, Hz) | J (Hz) | |||
| Ser201 | Amide carbonyl | 172.5c | |||
| α | 4.599 | dd | 4.3, 3.7 | 55.53 | |
| β | 4.055 | dd | 10.0, 4.3 | 67.67 | |
| 3.732 | dd | 10.0, 3.7 | |||
| α-l-Rhap 1 | 1 | 4.888 | br s (4.5) | 99.81 | |
| 2 | 3.977 | br s (7.2) | 79.90 | ||
| 3 | 3.780 | dd | 9.7, 3.1 | 71.66 | |
| 4 | 3.440 | dd | 9.7, 9.6 | 73.71 | |
| 5 | 3.541 | dq | 9.6, 6.0 | 70.84 | |
| 6 | 1.273 | d | 6.0 | 18.51 | |
| α-l-Rhap 2 | 1 | 4.979 | br s (4.5) | 103.55 | |
| 2 | 4.264 | br dd | 3.1, 1.6 | 71.38 | |
| 3 | 3.900 | dd | 9.8, 3.1 | 81.13 | |
| 4 | 3.591 | dd | 9.8, 9.8 | 72.83 | |
| 5 | 3.756 | dq | 9.8, 6.1 | 71.04 | |
| 6 | 1.271 | d | 6.1 | 18.39 | |
| β-d-Quip4N (4-amino-4,6-dideoxy-β-d-glucopyranosyl) | 1 | 4.726 | d | 8.0 | 105.20 |
| 2 | 3.126 | dd | 9.2, 8.0 | 84.94 | |
| 3 | 3.517 | dd | 10.2, 9.2 | 74.50 | |
| 4 | 3.619 | dd | 10.2, 10.0 | 58.26 | |
| 5 | 3.535 | dq | 10.0, 6.0 | 72.56 | |
| 6 | 1.199 | d | 6.0 | 18.64 | |
| 2-O-Me | 3.620 | s | 61.77 | ||
| N-(3-hydroxy-1-oxobutyl) | 1′ | 2.402 | dd | 14.1, 7.9 | 176.2c |
| 2′ | 2.422 | dd | 14.1, 5.5 | 46.87 | |
| 3′ | 4.188 | ddq | 7.9, 5.5, 6.3 | 66.73 | |
| 4′ | 1.218 | d | 6.3 | 23.77 | |
Obtained at 800.33 MHz for 1H and 125.76 MHz for 13C in D2O at 298 K. Numbers of rhamnosyl residues are based on the order from the reducing end.
s, singlet; d, doublet; t, triplet; q, quartet; br, broad; W1/2, width at half height.
Read from a position of an HMBC cross peak.