Table 1.
unit | C/H no | δ Ca | δH (J in Hz)b | COSYb | HMBCb |
---|---|---|---|---|---|
Br-Hmoya | 1 | 170.8, C | |||
2 | 42.4, CH | 3.11, br q (7.4) | H-3, H3-9 | 1, 3, 4, 9 | |
3 | 76.4, CH | 4.85, dt (10.2, 2.5) | H-2, H-4a, H-4b | 1, 1 (N-Me-Val-1) | |
4a | 27.4, CH2 | 2.06, m | H-3, H-4b, H-5a, H-5b | 5, 6 | |
4b | 1.59, m | H-3, H-4a, H-5a, H-5b | |||
5a | 25.0, CH2 | 1.60, m | H-4a, H-4b, H-5b, H2-6 | 7, 8 | |
5b | 1.41, m | H-4a, H-4b, H-5a, H2-6 | 6, 8 | ||
6 | 19.2, CH2 | 2.23, m | H-5a, H-5b | 7, 8 | |
7 | 38.4, C | ||||
8 | 79.3, C | ||||
9 | 14.1, CH3 | 1.25, d (7.4) | H-2 | 1, 2, 3 | |
N-Me-Val-1 | 1 | 170.6, C | |||
2 | 65.0, CH | 3.93, d (10.3) | H-3 | 1, 3, 4, N-Me, 1 (Pro) | |
3 | 28.3, CH | 2.30, m | H-2, H3-4, H3-5 | 2, 4, 5 | |
4 | 19.56, CH3 | 0.98, d (6.6) | H-3 | 2 | |
5 | 19.51, CH3 | 0.91, d (6.6) | H-3 | 2 | |
N-Me | 28.6, CH3 | 3.00, s | 2, 1 (Pro) | ||
Pro | 1 | 172.1, C | |||
2 | 57.3, CH | 4.94 dd (8.9, 4.5) | H-3a, H-3b | 1, 3, 4, 1 (Hmpa) | |
3a | 29.5, CH2 | 2.30, m | H-2, H-3b, H-4a | 1, 2, 5 | |
3b | 1.79, m | H-2, H-3a, H-4a | 1, 2, 5 | ||
4a | 24.9, CH2 | 2.03, m | H-3a, H-3b, H-4b, H-5a, H-5b | 2, 3, 5 | |
4b | 1.98, m | H-4a, H-5a, H-5b | 2, 3, 5 | ||
5a | 47.3, CH2 | 3.84, dt (−17.0, 7.1) | H-4a, H-4b, H-5b | 2, 3, 4 | |
5b | 3.61, dt (−17.0, 7.1) | H-4a, H-4b, H-5a | 3, 4 | ||
Hmpa | 1 | 165.9, C | |||
2 | 76.1, CH | 4.90, d (9.1) | H-3 | 1, 3, 4, 5, 1 (N-Me-Val-2) | |
3 | 35.7, CH | 1.97, m | H-2, H3-6 | ||
4a | 24.81, CH2 | 1.54, m | H-4b, H3-5 | ||
4b | 1.13, m | H-4a, H3-5 | |||
5 | 10.5, CH3 | 0.87, t (7.3) | H-4a, H-4b | 3, 4 | |
6 | 13.8, CH3 | 1.01, d (6.8) | H-3 | 2, 3, 4 | |
N-Me-Val-2 | 1 | 169.6, C | |||
2 | 66.0, CH | 4.15, d (9.5) | H-3 | 1, 3, 5, N-Me, 1(Val) | |
3 | 28.5, CH | 2.27, m | H-2, H3-4, H3-5 | 1 | |
4 | 20.4, CH3 | 1.00, d (7.0) | H-3 | 2 | |
5 | 20.2, CH3 | 1.11, d (7.0) | H-3 | 2, 3 | |
N-Me | 30.0, CH3 | 2.94, s | 2, 1 (Val) | ||
Val | 1 | 173.4, C | |||
2 | 52.8, CH | 4.70, dd (8.7, 6.5) | H-3, NH | 1, 3, 4, 5, 1 (Br-Hmoya) | |
3 | 32.1, CH | 1.96, m | H-2, H3-4, H3-5 | 5 | |
4 | 20.3, CH3 | 0.95, d (6.7) | H-3 | 2, 3, 5 | |
5 | 17.5, CH3 | 0.88, d (6.7) | H-3 | 2, 3 | |
NH | 6.25, d (8.7) | H-2 | 1, 1 (Br-Hmoya) |
100 MHz
600 MHz