Table 1.
1Ha, δ, mult (J, Hz) | 13Cb δ (mult) | COSYa | NOESYa | HMBCa | |
---|---|---|---|---|---|
1 | |||||
2 | 3.49, m | 55.8 (CH) | 9, 3 | 3, 4ax | 9 |
3 | 5.04, q (2.8) | 67.8 (CH) | 2, 4ax, 4eq | 2,4ax, 4eq, 9 | 1”, 4, 5, 9 |
4ax | 2.48, d (15.6) | 28.9 (CH2) | 3, 4eq, 5 | 3, 4eq, 4a, 1’ | 2, 3, 8a, 4a, 5 |
4eq | 1.63, mc | 3, 4ax | 3, 4ax, 4a, | 8a, 4a, 5 | |
4a | 1.54, md | 37.5 (CH) | 4eq, 5 | 4ax, 4eq, 8a, 5, 6ax | 3, 8a, 5, |
5 | 1.95, m | 34.5 (CH) | 4a, 6ax, | 4a, 1’, 2’, 6ax | 4a, 6, 1’, |
6ax | 0.81, qd (12.6, 3.3) | 31.2 (CH2) | 5, 6eq, 7eq, 7ax | 4a, 5, 6eq, 7ax, 7eq, 8ax | 4a, 5, 7,8 |
6eq | 1.87, brd (12.6) | 6ax, 7ax, 7eq | 5, 6ax, 1’, 2’ | 4a, 8, | |
7eq | 1.54, md | 19.9 (CH2) | 6eq, 7ax, | 6ax, 8eq, 7ax | 8a, 5 |
7ax | 1.74, qt (13.5, 3.3) | 6eq, 6ax, 7eq, 8eq, 8ax | 6ax, 8eq, 7eq, | 6, 8 | |
8αx | 1.64, mc | 29.3 (CH2) | 8a, 8eq, 7ax | 6ax, 8a, 8eq, | 8a, 4a, 6, 7 |
8eq | 2.01, d (14.5) | 8a, 8ax, 7eq | 7ax, 7eq, 8ax | 8a, 4a, 6, 7 | |
8a | 3.46, m | 57.4 (CH) | 4a, 8ax, 8eq | 4ax, 4a, 8ax, 8eq | 7 |
9 | 1.31, mh | 14.8 (CH3) | 2 | 3, 2” | 2, 3 |
1” | 164.6 (Cq) | ||||
2” | 5.74, d (14.9) | 111.7 (CH) | 4” | 4” | 2, 1”, 3” |
3” | 8.07, d (14.9) | 150.0 (CH) | 3” | 3” | 1”, 2”, 5” |
4” | |||||
5” | 2.33, s, 3H | 14.2 (CH3) | 3” | ||
1’ | 0.92, mf 1.36, me |
33.1 (CH2) | 2’ | 4eq, 5, 6eq | 5, 3’, 2’ |
2’ | 1.07, m 1.31, me |
26.1 (CH2) | 1’, 3’ | 5, 6eq | 1’, 3’ |
3’ | 1.20, mg | 30.3 (CH2) | 2’, 4’ | 1’, 4’, 5’ | |
4’ | 1.24, mg | 30.0 (CH2) | 3’ | 6’, 5’ 3’, | |
5’ | 1.26, mg 1.36, me |
25.8 (CH2) | 7’, | ||
6’ | 1.39, me | 37.7 (CH2) | 7’ | ||
7’ | 3.57, m | 71.8 (CH) | 6’, 8’ | 5’, 9’ | |
8’ | 1.39, me | 39.9 (CH2) | 7’, 9’ | ||
9’ | 1.35, me 1.44, me |
19.3 (CH2) | 8’, 10’ | 7’, 8’ | |
10’ | 0.91, t (6.8)f | 14.3 (CH3) | 9’ | 8’, 9’ | |
NH | 8.23, bs |
600 MHz, in the presence of Et2NH•TFA buffer (~20 mM).
, 150 MHz, multiplicities assigned by APT and edited HSQC.
overlapped signals. i signal overlapped.