Table 1.
2a |
3 |
4 |
|||||
---|---|---|---|---|---|---|---|
positionb | δH (J in Hz) | δ C | δH (J in Hz) | δ C | δH (J in Hz) | δ C | |
Acyl | 1 | 166.1, s | 165.3, s | 165.5, s | |||
2 | 6.98, 1H, d (16.0) | 122.2, d | 6.88, 1H, d (15.7) | 123.3, d | 6.71, 1H, d (15.7) | 123.3, d | |
3 | 7.91. 1H, d (16.0) | 140.0, d | 7.54, 1H, d (15.7) | 137.1, d | 7.55, 1H, d, 15.7) | 137.0, d | |
1′ | 133.6, s | 138.0, s | 138.0, s | ||||
2′ | 7.56, 1H, d (7.80) | 126.3, d | 7.62, 1H, d (6.86) | 125.9, d | 7.58, 1H, d (7.63) | 125.9, d | |
3′ | 7.18, 1H, t, (7.60) | 127.0, d | 7.36, 1H, t (7.00) | 129.0, d | 7.37, 1H, t (7.21) | 129.4, d | |
4′ | 7.29, 1Hc | 128.9, d | 7.33, 1H, t (6.72) | 127.4, d | 7.33, 1H, t (7.35) | 127.8, d | |
5′ | 7.20, 1H, d (7.80) | 129.9, d | 7,19, 1He | 129.7, d | 7.20, 1Hf | 130.5, d | |
6′ | 138.4, s | 137.0, s | 137.0, s | ||||
1″ | 6.55, 1H, d (11.4) | 126.9, d | 6.53, 1H, d (11.5) | 126.9, d | 6.51, 1H, d (10.8) | 127.4, d | |
2″ | 5.80, 1H, dt (11.5, 7.40) | 134.9, d | 5.79, 1H, m | 134.1, d | 5.78, 1H, m | 134.1, d | |
3″ | 2.00, 2H, m | 30.5, t | 1.97, 2H, m | 30.0, t | 1.98, 2H, m | 29.0, t | |
4″ | 1.35, 2H, m | 22.7, t | 1.36, 2H, m | 22.1, t | 1.36, 2H, m | 22.9, t | |
5″ | 0.80, 3H, t (7.50) | 13.8, q | 0.90, 3H, t (7.33) | 13.6, q | 0.81, 3H, t (7.28) | 13.7, q | |
1Ser/1Thr | NH | 7.65, 1H, d (7.80) | 8.58, 1H, brs | 8.64, 1H, brs | |||
α | 5.45, 1H, m | 50.9, d | 5.01, 1H, m | 52.9, d | 5.05, 1H, m | 51.3, d | |
β | 4.43, 1H, m | 63.8, t | 4.11, 1H, m | 66.6, d | 3.56, 1H, m | 61.3, t | |
4.68, 1H, m | 3.80, 1H, m | ||||||
γ | 1.05, 3H, brs | 20.0, q | |||||
CO | 169.5, s | 170.9, s | 170.9, s | ||||
2ΔMeTyr | NMe | 3.57, 3H, s | 40.4, q | 2.88, 3H, s | 34.0, q | 2.86. 3H, s | 33.4, q |
α | 138.8, s | 130.7, s | 129.4, s | ||||
β | 6.84, 1H, s | 128.2, d | 6.60, 1H, s | 131.6, d | 6.70, 1H, s | 130.7, d | |
1 | 131.0, s | 123.5, s | 123.3, s | ||||
2,6 | 7.29, 2Hc | 129.9, d | 7.28, 2H, d (7.63) | 129.3, d | 7.19, 2Hf | 130.7, d | |
3,5 | 7.05, 2Hd | 121.9, d | 6.67, 2H, d (7.07) | 115.1, d | 6.67, 2H, d (7.98) | 115.2, d | |
4 | 150.9, s | 158.4, s | 158.6, s | ||||
CO | 166.0, s | 164.9, s | 165.3, s | ||||
CO (Ac) | 169.6, s | ||||||
Me (Ac) | 2.30, 3H, s | 21.1, q | |||||
3Leu | NH | 8.08, 1H, d (8.20) | 7.28, 1H, brs | 7.35, 1H, d (9.35) | |||
α | 4.45, 1H, m | 51.1, d | 4.35, 1H, m | 51.5, d | 4.39, 1H, m | 51.5, d | |
β | 1.28, 1H, m | 38.0, t | 1.20, 2H, m | 40.0, t | 1.20, 2H, m | 39.2, t | |
1.64, 1H, m | |||||||
γ | 1.00, 1H, m | 24.2, d | 1.15, 1H, m | 23.9, d | 0.85, 1H, m | 24.0, d | |
δ | 0.71, 3H, d (6.60) | 23.0, q | 0.70, 3H, brs | 21.7, q | 0.73, 3H, d (6.20) | 22.1, q | |
0.79, 3H, d (7.10) | 21.5, q | 0.70, 3H, brs | 22.7, q | 0.73, 3H, d (6.20) | 22.5, q | ||
CO | 170.9, s | 172.4, s | 173.2, s | ||||
4Phe | NH | 7.94, 1H, d (8.10) | 8.49, 1H, brs | 8.44, 1H, brs | |||
α | 4.70, 1H, m | 54.9, d | 4.72, 1H, m | 53.9, d | 4.74, 1H, m | 53.8, d | |
β | 2.79, 1H, m | 36.7, t | 2.71, 1H, m | 38.0, t | 2.72, 1H, m | 37.4, t | |
3.13, 1H, dd (13.8, 8.20) | 3.05, 1H, m | 3.05, 1H, m | |||||
1 | 137.2, s | 137.1, c | 137.0, s | ||||
2,6 | 7.12, 2H, d (7.50) | 129.2, d | 7.20, 2He | 130.7, d | 7.30, 2H, d (7.14) | 129.7, d | |
3,5 | 6.99, 2H, t (7.70) | 128.4, d | 7.22, 2He | 127.8, d | 7.22, 2Hf | 129.0, d | |
4 | 7.05, 1Hd | 126.9, d | 7.15, 1H, t (6.51) | 126.0, d | 7.14, 1H, t (7.28) | 126.9, d | |
CO | 173.4, s | 170.9, s | 170.9, s | ||||
5allo Thr | NH | 7.28, 1H, d (8.40) | 8.10, 1H, brs | 8.07, 1H, brd (6.23) | |||
α | 4.93, 1H, dd (8.10, 3.60) | 56.0, d | 4.04, 1H, m | 58.5, d | 4.02, 1H, m | 58.8, d | |
β | 5.28, 1H, m | 69.1, d | 3.65, 1H, m | 67.0, d | 3.68, 1H, m | 67.6, d | |
γ | 1.18, 3H, d (6.60) | 15.1, q | 0.98, 3H, brs | 20.0, q | 0.97, 3H, brs | 20.1, q | |
CO | 168.1, s | 170.4, s | 170.5, s | ||||
CO (Ac) | 170.5, s | ||||||
Me (Ac) | 1.79, 3H, s | 20.7, q | |||||
6Asn | NH | 7.65, 1H, d (7.80) | |||||
α | 4.86, 1H, td (9.00, 4.40) | 49.3, d | |||||
β | 2.63, 1H, dd (15.2, 4.30) | 36.0, t | |||||
2.81, 1H, m | |||||||
γCO | 173.1, s | ||||||
CO | 173.4, s | ||||||
7Ser | NH | 7.19, 1H, d (7.21) | |||||
α | 4.26, 1H, dd (11.3, 5.30) | 52.7, d | |||||
β | 4.42, 1H, m | 62.4, t | |||||
4.58, 1H, dd (13.2, 7.70) | |||||||
CO | 170.2, s | ||||||
CO (Ac) | 170.9, s | ||||||
Me (Ac) | 2.06, 3H, s | 20.8, q |
Assignments were based on COSY, HSQC, HMBC, and NOSEY experiments
Numbering followed literature precedence7
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