Table 3.
position | 1H δ; mult. (J Hz) | 13C δ; type | gHMBC | gCOSY | 15N δ | |
---|---|---|---|---|---|---|
OAc-Gln1 | 1 | 1.80; s | 22.5; CH3 | C-2 | ||
2 | 169.0; C | |||||
NH | 7.93; d (8.5) | C-2, C-7 | H-3 | 124.3 | ||
3 | 4.31; dt (5.0, 8.5) | 52.1; CH | C-7 | Gln NH, H-4b | ||
4 | 1.80; m, 1.66; ddt (13, 8.5, 5.0) | 28.5; CH2 | H-3 | |||
5 | 2.03; m | 31.6; CH2 | ||||
6 | 173.7; C | |||||
NH2 | 7.26; s, 6.74; s | C-5, C-6 | 115.4 | |||
7 | 171.4; C | |||||
Ile2 | NH | 8.14; d(8.5) | C-7, C-13 | H-10 | 124.3 | |
8 | 4.52; t (9.0) | 52.5; CH | Ile NH, H-9 | |||
9a | 1.80; m | 36.0; CH | H-8 | |||
10b | 1.44; m, 1.06; m | 24.0; CH2 | ||||
11c | 0.77; m | 10.6; CH3 | ||||
12d | 0.77; m | 14.9; CH3 | ||||
13 | 172.6; C | |||||
MeLeu3 | 14e | 2.94; s | 31.1; CH3 | C-15 | 115.4 | |
15 | 5.07; dd (4.5, 12.0) | 53.8; CH | C-13, C-16, C-20 | H-16a | ||
16 | 1.78; m, 1.55; ddd (4.5, 11.0, 14.5) | 36.4; CH2 | H-15 | |||
17 | 1.80; m | 24.5; CH | ||||
18f | 0.77; m | 21.2; CH3 | ||||
19f | 0.77; m | 20.8; CH3 | ||||
20 | 169.9; C | |||||
Ile4 | NH | 8.31; d (8.0) | C-20 | H-21 | 115.4 | |
21 | 4.46; dd (8.5, 9.5) | 52.7; CH | C-20, C-22 | Ile NH, H-22 | ||
22 | 1.80; m | 35.5; CH | H-21 | |||
23b | 1.44; m, 1.06 m | 24.0; CH2 | ||||
24c | 0.77; m | 10.5; CH3 | ||||
25d | 0.77; m | 14.9; CH3 | ||||
26g | 170.3; C | |||||
MeVal5 | 27e | 3.02; s | 30.7; CH3 | C-28 | 116.2 | |
28 | 5.10; d (11.0) | 57.2; CH | C-29, C-32 | H-29 | ||
29 | 2.19; dq (6.5, 11.0) | 26.7; CH | H-28 | |||
30h | 0.77; m | 18.8; CH3 | ||||
31h | 0.77; m | 17.9; CH3 | ||||
32 | 172.3; C | |||||
MeIle6 | 33e | 2.94; s | 30.0; CH3 | C-32 | 117.8 | |
34 | 5.20; d (11.0) | 55.5; CH | H-35 | |||
35a | 2.03; m | 32.6; CH | H-34 | |||
36b | 1.39; m, 1.30; m | 23.6; CH2 | ||||
37c | 0.77; m | 10.4; CH3 | ||||
38d | 0.77; m | 14.8; CH3 | ||||
39 | 172.1; C | |||||
MeIle7 | 40e | 3.08; s | 29.9; CH3 | C-39, C-41 | 116.0 | |
41 | 4.78; d (11.0) | 58.8; CH | C-39, C-42, C-46 | H-42 | ||
42 | 1.80; m | 32.2; CH | H-41 | |||
43b | 1.39; m, 1.13; m | 23.4; CH2 | ||||
44c | 0.77; m | 10.4; CH3 | ||||
45d | 0.77; m | 14.6; CH3 | ||||
46 | 169.9; C | |||||
MeIle8OH | 47e | 2.94; s | 29.9; CH3 | C-46, C-48 | 117.4 | |
48 | 5.17; d (11.0) | 55.2; CH | C-46 | H-49 | ||
49a | 2.03; m | 32.6; CH | H-48 | |||
50b | 1.39; m, 1.30; m | 23.2; CH2 | ||||
51c | 0.77; m | 10.2; CH3 | ||||
52d | 0.77; m | 14.6; CH3 | ||||
53g | 170.1; C | |||||
OH | n.o. |
Interchangeable carbons
Interchangeable carbons
Interchangeable carbons
Interchangeable carbons
Interchangeable carbons
Interchangeable carbons
Interchangeable carbons
Interchangeable carbons
n.o.: not observed; low-field diastereotopic protons are labeled “a”, high-field diastereotopic protons are labeled “b”.