Table 2.
1H- and 13C-NMR data for champacyclin (1a) in d6-DMSO on a 600 MHz NMR spectrometer at 30 °C.
| Amino Acid/Position | 1H NMR δ(1H) in ppm | 13C NMR δ(13C) in ppm (mult.) * | Amino Acid/Position | 1H NMR δ(1H) in ppm | 13C NMR δ(13C) in ppm (mult.) * |
|---|---|---|---|---|---|
| Lys(1) | Leu(5) | ||||
| C=O | − | n.d. | C=O | − | n.d. |
| NH | 7.40 | − | NH | 7.77 | − |
| Hα | 4.34 | 51.5, CH | Hα | 4.22 | 52.7, CH |
| Hβ/β′ | 1.55/1.40 | 31.6, CH2 | Hβ/β′ | 1.93/1.49 | 39.7, CH2 |
| Hγ/γ′ | n.d. | n.d. | Hγ | 1.72 | 24.1, CH |
| Hδ/δ′ | n.d. | n.d. | Hδ/δ′ | 0.96/0.89 | 22.9/21.4, CH2 |
| Hε/ε′ | n.d. | n.d. | |||
| NH2 | n.d. | n.d. | |||
| Ile(x) | Ile(6) | ||||
| C=O | − | n.d. | C=O | − | n.d. |
| NH | n.d. | − | NH | 6.91 | − |
| Hα | 4.15 | 57.1, CH | Hα | 4.05 | 57.7, CH |
| Hβ | 1.85 | 35.6, CH | Hβ | 1.82 | 35.5, CH |
| Hγ | 0.84 | 14.7, CH3 | Hγ | 0.80 | n.d. |
| Hγ′ | n.d. | n.d. | Hγ′ | 1.23/1.13 | 23.5, CH2 |
| Hδ | n.d. | n.d. | Hδ | n.d. | n.d. |
| Ile(3) | Ala(7) | ||||
| C=O | − | 171.4 | C=O | − | 172.4 |
| NH | 7.93 | − | NH | 7.78 | − |
| Hα | 3.78 | 57.7, CH | Hα | 4.28 | 47.7, CH |
| Hβ | 1.47 | 35.5, CH | Hβ/β′/β′′ | 1.25 | 18.4, CH3 |
| Hγ | 0.45 | 14.9, CH | |||
| Hγ′ | 1.22/0.83 | 24.1, CH2 | |||
| Hδ | 0.72 | 10.7, CH3 | |||
| Phe(4) | Ile(x) | ||||
| C=O | − | 171.0 | C=O | − | n.d. |
| NH | 8.40 | − | NH | n.d. | − |
| Hα | 4.33 | 54.8, CH | Hα | 4.14 | 57.9, CH |
| Hβ/β′ | 3.29/2.70 | 36.6, CH2 | Hβ | 1.85 | 35.6, CH |
| Hγ | − | 138.3, CH | Hγ | n.d. | n.d. |
| Hδ/δ′ | 7.20 | 129.4, CH | Hγ′ | 1.34/1.22 | 25.3, CH2 |
| Hε/ε′ | 7.26 | 128.1, CH | Hδ | n.d. | n.d. |
| Hζ | 7.36 | 126.3, CH |
n.d. = not determined; * = multiplicities were deduced from DEPT-HMQC.