TABLE 3.
Assignments of 13C and 1H NMR data for acetyl-glycylthricina
| Position | δC | δH (multiplicity; J in Hz) | 1H-1H COSY | 1H-13C HMBC |
|---|---|---|---|---|
| 1 | 173.0 | |||
| 2 | 56.3 | 4.31 (d, 14.1) | 3 | 1, 4 |
| 3 | 52.2 | 4.35 (dd, 14.1, 2.2) | 2 | |
| 4 | 62.1 | 4.62 (ddd, 5.6, 2.2, 1.2) | 5 | 2 |
| 5 | 49.3 | 3.78 (dd, 14.4, 5.6) | 4 | 1 |
| 3.36 (dd, 14.4, 1.2) | 1 | |||
| 6 | 164.2 | |||
| 7 | 79.8 | 5.12 (d, 9.6) | 8 | 6, 11 |
| 8 | 50.1 | 4.13 (dd, 9.6, 2.9) | 7 | 10, 14 |
| 9 | 66.9 | 4.12 (t, 2.9) | 10 | 8, 11 |
| 10 | 70.4 | 4.75 (dd, 3.5, 2.9) | 9 | 8, 13 |
| 11 | 73.4 | 4.26 (dt, 6.5, 3.5) | 12 | 7 |
| 12 | 60.5 | 3.70 (d, 6.5) | 11 | |
| 13 | 158.2 | |||
| 14 | 171.6 | |||
| 15 | 42.6 | 3.92 (s) | 14, 16 | |
| 16 | 175.0 | |||
| 17 | 21.8 | 2.06 (s) | 16 |
a
NMR assignment of acetyl-glycylthricin. 1H and 13C NMR spectra were recorded at 600 and 150 MHz, respectively, using the Varian NMR system 600 NB CL (Varian, Palo Alto, CA, USA). One- and two-dimensional experiments (double-quantum-filtered correlation spectroscopy [DQF-COSY] and constant-time heteronuclear multiple-bond connectivity [CT-HMBC]) were performed at ambient temperature, and the correlation positions are shown. The samples were dissolved in D2O, and the solvent peak was used as an internal standard (δH, 4.80 ppm).