Table 2.
Terpendole N (1) a | |||||||
Position | δCc, type | δHd (multi, J Hz) | HMBC | Position | δCc, type | δHd (multi, J Hz) | HMBC |
1-NH | - | 10.08 (s) | 2, 18, 19, 24 | 18 | 76.8, C | - | - |
2 | 180.2, C | - | - | 18-OH | - | 5.72 (s) | 18, 19 |
3 | 74.6, C | - | - | 19 | 128.9, C | - | - |
3-OH | - | 3.74 (s) | 3, 16, 25 | 20 | 136.7, C | - | - |
4 | 44.9, C | - | - | 21 | 121.9, CH | 6.81 (d, 7.6) | 19, 23 |
5 | 23.2, CH2 | 1.15–1.21 (m) | 4 | 22 | 128.8, CH | 7.11 (t, 7.6) | 20, 24 |
1.92 (m) | 23 | 107.5, CH | 6.63 (d, 7.6) | 19, 21 | |||
6 | 28.1, CH2 | 1.32 (m) | 4, 7, 12 | 24 | 141.7, C | - | - |
1.88 (m) | 25 | 19.5, CH3 | 1.08 (s) | 3, 16 | |||
7 | 70.5, CH | 4.02 (dd, 10.2, 7.4) | 6, 11, 12 | 26 | 16.7, CH3 | 0.59 (s) | 4, 5, 13 |
27 | 74, C | - | - | ||||
9 | 70.9, CH | 3.34 (d, 9.6) | 27, 28, 29 | 28 | 16.7, CH3 | 1.14 (s) | 9, 27, 29 |
29 | 28.3, CH3 | 1.073 (s) | 9, 27, 28 | ||||
10 | 70.1, CH | 3.92 (d, 9.6) | - | 31 | 92, CH | 5.42 (d, 6.4) | 10, 27, 34 |
11 | 59.1, CH | 3.33 (br s) | 7, 9, 12 | 33 | 122.5, CH | 5.05 (br d, 6.4) | 35, 36 |
12 | 66.8, C | - | - | 34 | 137.5, C | - | - |
13 | 75.9, C | - | - | 35 | 18.4, CH3 | 1.61 (d, 1.2) | 34, 36 |
13-OH | - | 4.18 (s) | 4, 13, 14 | 36 | 25, CH3 | 1.63 (s) | 34, 35 |
14 | 25.5, CH2 | 0.81–0.90 (m) | 4 | 37 | 29.7, CH2 | 2.87 (m) | 19, 20, 21, 39 |
1.04–1.08 (m) | 3.03 (m) | ||||||
15 | 23.7, CH2 | 1.10 (d, 4.8) | 17 | 38 | 62.9, CH | 3.02 (m) | 20 |
1.27 (s) | 39 | 57.8, C | - | - | |||
16 | 37.5, CH | 1.27–1.34 (m) | - | 40 | 18.9, CH3 | 1.27 (s) | 41 |
17 | 37.1, CH2 | 1.68 (dd, 12.6, 10.6) | 2, 3, 15, 18 | 41 | 24.7, CH3 | 1.23 (s) | 38, 39, 40 |
2.29 (d, 12.6) | |||||||
Terpendole O (2) a | |||||||
Position | δCc, type | δHd (multi, J Hz) | HMBC | Position | δCc, type | δHd (multi, J Hz) | HMBC |
1-NH | - | 10.69 (s) | 2, 18, 19, 24 | 18 | 114.3, C | - | - |
2 | 152.3, C | - | - | 18-OH | - | - | - |
3 | 49.9, C | - | - | 19 | 124.1, C | - | - |
3-OH | - | - | - | 20 | 128.0, C | - | - |
4 | 42.1, C | - | - | 21 | 118.2, CH | 6.71 (d, 7.2) | 19, 23 |
5 | 25.5, CH2 | 1.67 (br d, 6.4) | 26 | 22 | 119.5, CH | 6.86 (t, 7.6) | 20, 24 |
2.42 (br d, 6.4) | 23 | 110.1, CH | 7.12 (d, 8.0) | 19, 21 | |||
6 | 28.53, CH2 | 2.12 (br m) | - | 24 | 139.7, C | - | - |
25 | 16, CH3 | 1.16 (s) | 2, 3, 4 | ||||
7 | 70.6, CH | 4.26 (t, 8.8) | 9, 11 | 26 | 18, CH3 | 1.02 (s) | 3, 4, 5, 13 |
27 | 74.1, C | - | - | ||||
9 | 71, CH | 3.40 (d, 9.6) | 7, 27, 28, 29 | 28 | 16.7, CH3 | 1.22 (s) | 9, 27, 29 |
29 | 28.2, CH3 | 1.12 (s) | 9, 27, 28 | ||||
10 | 70.1, CH | 4.04 (d, 9.6) | 27 | 31 | 91.9, CH | 5.50 (d, 6.4) | 10, 27, 34 |
11 | 58.9, CH | 3.50 (br. s) | 7, 9, 12 | 33 | 122.5, CH | 5.10 (d, 6.4) | 35, 36 |
12 | 67.0, C | - | - | 34 | 137.4, C | - | - |
13 | 76.5, C | - | - | 35 | 18.3, CH3 | 1.63 (d, 0.8) | 33, 34, 36 |
13-OH | - | 4.50 (s) | 4 | 36 | 25.0, CH3 | 1.64 (s) | 33, 34, 35 |
14 | 28.38, CH2 | 1.46 (br m) | - | 37 | 32.3, CH2 | 2.93 (m) | 21 |
1.52 (br s) | 3.01 (dd, 16, 8.4) | ||||||
15 | 20.3, CH2 | 1.46 (br m) | - | 38 | 63.4, CH | 2.93 (m) | 20, 21 |
1.80 (br m) | 39 | 57.9, C | - | - | |||
16 | 49.6, CH | 2.71 (br m) | - | 40 | 18.7, CH3 | 1.32 (s) | 38, 39, 41 |
17 | 28.58, CH2 | 2.45 (br s) | 2, 3, 18 | 41 | 24.6, CH3 | 1.23 (s) | 38, 39, 40 |
2.71 (br m) | |||||||
Terpendole P (3) b | |||||||
Position | δCc, type | δHd (multi, J Hz) | HMBC | Position | δCc, type | δHd (multi, J Hz) | HMBC |
1-NH | - | 10.81 (s) | 2, 18, 19, 24 | 18 | 114.7, C | - | - |
2 | 150.6, C | - | - | 19 | 124.1, C | - | - |
3 | 38.3, C | - | - | 20 | 117.8, CH | 7.26 (d, 7.8) | 18, 22 |
3-OH | - | - | - | 21 | 118.4, CH | 6.88 (td, 7.8, 1.2) | 19, 23 |
4 | 48.3, C | - | - | 22 | 119.5, CH | 6.93 (td, 7.8, 1.2) | 20, 24 |
5 | 27.9, CH2 | 2.05 (m) | 3, 4, 7, 13 | 23 | 111.7, CH | 7.24 (d, 7.8) | 19, 21 |
24 | 140.1, C | - | - | ||||
6 | 28.2, CH2 | 1.75 (m)2.30 (m) | - | 25 | 16.2, CH3 | 0.99 (s) | 2, 3, 4, 16 |
26 | 18, CH3 | 1.12 (s) | 3, 4, 5, 13 | ||||
7 | 70.6, CH | 3.86 (m) | 9, 12 | 27 | 76.9, C | - | - |
28 | 21.4, CH3 | 1.17 (s) | 9, 27, 29 | ||||
9 | 75.5, CH | 3.25 (d, 9.0) | 7, 11, 27, 28, 29 | 29 | 23.9, CH3 | 1.16 (s) | 9, 27, 28 |
31 | 58.1, CH2 | 3.87 (m) | 10, 27, 34 | ||||
10 | 65.5, CH | 3.89 (m) | - | 3.91 (m) | |||
10-OH | - | 4.78 (d, 4.2) | 9, 10, 11 | 33 | 122.1, CH | 5.18 (dd, 7.0, 1.2) | 35, 36 |
11 | 63.1, CH | 3.32 (s) | 9, 10, 12 | 34 | 134.5, C | - | - |
12 | 62.9, C | - | - | 35 | 17.7, CH3 | 1.58 (s) | 34, 36 |
13 | 66.9, C | - | - | 36 | 25.3, CH3 | 1.65 (s) | 33, 34, 35 |
14 | 54.7, CH | 3.19 (d, 5.4) | 12, 13 | ||||
15 | 24.5, CH2 | 2.02 (m) | 13, 17 | ||||
1.85 (m) | |||||||
16 | 45, CH | 2.63 (m) | 2, 3, 4, 18 | ||||
17 | 26.7, CH2 | 2.17 (m) | 2, 3, 15, 18 | ||||
2.62 (m) |
a 13C (100 MHz) and 1H (400 MHz) spectra were taken on an NMR 400 MHz spectrometer (Agilent). b13C (150 MHz) and 1H (600 MHz) spectra were taken on an NMR 600 MHz spectrometer (Bruker). Chemical shifts are shown with reference to c DMSO-d6 as δ 39.5, d DMSO- d6 as δ 2.48. Multiplicity of signals as follows: s = singlet, d = doublets, dd = double doublets, t = triplet, m = multi. Coupling constants (Hz) were determined by the 1H-1H decoupling experiments.