Table 1. NMR data for found compound (1 in CD3CN (600 MHz).
δH(J in Hz) | δC, mult. | COSYa | HMBCb | ||
---|---|---|---|---|---|
Amoa | 1 | 174.8, C | |||
2 | 2.70, qd (7.5, 4.1) | 44.9, CH | 3, 9 | 1, 3, 4, 9 | |
3 | 3.97, m | 52.8, CH | 2, 4b, 9, NH | 1, 2, 4 | |
4a | 1.60, m | 29.7, CH2 | 4b, 5a, 5b | 3, 5, 6 | |
4b | 1.11, m | 4a, 5a | 3, 5, 6 | ||
5a | 1.28, m | 32.9, CH2 | 4a, 4b, 5b | 4, 7 | |
5b | 1.13, m | 4a, 5a | 4, 7 | ||
6a | 1.28, m | 27.1, CH2 | 6b | ||
6b | 1.12, m | 6a | |||
7 | 1.27, m | 23.8, CH2 | 8 | 5, 6 | |
8 | 0.86, d (6.2) | 14.8, CH3 | 7 | ||
9 | 1.13, d (6.9) | 15.7, CH3 | 2 | 1, 2 | |
NH | 8.93, d (8.9) | 3 | 10 | ||
Ala | 10 | 172.7, C | |||
11 | 4.35, dq (8.3, 6.9) | 52.4, CH | 12, NH | 10, 12, 13 | |
12 | 1.25, d (6.8) | 20.8, CH3 | 11 | 11, 10 | |
NH2 | 6.57, d (8.3) | 11 | 11, 12, 13 | ||
N-Me-Phe | 13 | 170.5, C | |||
14 | 5.52, dd (10.3, 5.5) | 58.4, CH | 15a, 15b | 13, 15, 16, 22, 23 | |
15a | 3.26, dd (-15.0, 5.5) | 34.3, CH2 | 14, 15b | 13, 14, 16, 17, 21 | |
15b | 2.90, dd (-15.0, 10.3) | 14, 15a | 13, 14, 16, 17, 21 | ||
16 | 139.6, C | ||||
17 | 7.18, d (6.9) | 130.2, CH | 19, 21 | 15, 18, 19 | |
18 | 7.24, m | 129.5, CH | 17, 19, 21 | 16, 17 | |
19 | 7.18, t (6.9) | 127.6, CH | 18, 20 | 17, 18, 20, 21 | |
20 | 7.24, m | 129.5, CH | 17, 19, 21 | 16, 21 | |
21 | 7.18, d (6.9) | 130.2, CH | 18, 20 | 15, 19, 20 | |
22 | 2.96, s | 32.4, CH3 | 14, 23 | ||
Pro | 23 | 175.3, C | |||
24 | 4.51,dd (6.9, 3.4) | 59.6, CH | 25a, 25b | 23, 25 | |
25a | 1.80, m | 28.8, CH2 | 24, 25b, 26b | 26, 27 | |
25b | 1.57, m | 24, 25a, 26a, 26b | 23, 24, 26 | ||
26a | 2.06, m | 27.6, CH2 | 25b, 26b, 27a, 27b | 24, 25 | |
26b | 1.87, m | 25a, 25b, 26a, 27a, 27b | 25, 27 | ||
27a | 3.70, dd (9.0, 9.0) | 48.2, CH2 | 26a, 26b, 27b | 24, 25, 28 | |
27b | 3.44, m | 26a, 26b, 27a | 26 | ||
Hmpa | 28 | 170.0, C | |||
29 | 5.23, d (2.7) | 78.3, CH | 30 | 1, 28, 30, 31, 33 | |
30 | 2.15, m | 35.4, CH | 29, 31a, 31b, 33 | 31, 32, 33 | |
31a | 1.38, m | 24.3, CH2 | 31b, 32 | 29, 30, 32, 33 | |
31b | 1.17, m | 30, 31a, 32 | 30, 32, 33 | ||
32 | 0.87, t (6.9) | 12.5, CH3 | 31a, 31b | 30, 31 | |
33 | 1.01, d (6.9) | 16.4, CH3 | 30 | 29, 30, 31 |
COSY correlations are from proton stated to indicated proton.
HMBC correlations are from proton stated to the indicated carbon.