C Atom | Atom | 13C Shifta | Carbon Multiplicity from 13C- and 2D 1H, 13C-COSY (HSQC) Spectrum | 1H Shifta and 1H, 13C-COSY (HSQC)b Correlations | 1H Multiplicity | 1H-1H COSY Correlationsc | 1H, 13C Long-Range Correlations from HMBC Spectrum, 1H Shifts,d |
---|---|---|---|---|---|---|---|
ppm | ppm | ||||||
24 | C | 166.4 | Cq | 7.98 | |||
3 | C | 159.9 | Cq | 8.04 | |||
13 | C | 156.3 | Cq | 10.78/8.04/7.37 | |||
19 | C | 155.2 | Cq | 7.39 | |||
5 | C | 152.0 | Cq | 7.54 | |||
6 | C | 141.1 | Cq | 7.98 | |||
21 | C | 132.5 | CH | 7.39 | t | 6.98/6.86 | |
15 | C | 131.4 | CH | 7.37 | td | 7.00/7.02 | |
23 | C | 131.0 | CH | 7.54 | dd | 6.98 | |
9 | C | 130.6 | Cq | 7.55 | |||
8/10 | C | 130.3 | CH | 7.98 | dm | 7.55 | |
17 | C | 126.7 | CH | 8.04 | dd | 7.00 | |
7/11 | C | 123.3 | CH | 7.55 | dm | 7.98 | |
16 | C | 119.7 | CH | 7.00 | t | 8.04/7.37 | |
22 | C | 119.4 | CH | 6.98 | t | 7.54/7.39 | |
14 | C | 117.0 | CH | 7.02 | d | 7.37 | 10.78 |
20 | C | 116.1 | CH | 6.86 | d | 7.39 | |
18 | C | 114.4 | Cq | 6.86 | |||
12 | C | 113.6 | Cq | 10.78 | |||
13-OH | 10.78 | s | |||||
19-OH | 10.04 | sbr | |||||
COOH |
|
|
| 13.19 | sbr |
|
|
s, singlet; d, doublet; t, triplet; q, quartet; br, broad
↵ a Chemical shift reference; internal to the middle line of the DMSO-d6 NMR solvent signal: 1H: δ = 2.500 ppm; 13C: δ = 39.52 ppm; concentration: 30 mg in 0.7 ml of DMSO-δ6
↵ b 1H, 13C-COSY HSQC experiment: heteronuclear correlated spectroscopy. Heteronuclear single quantum coherence experiment with 1H detection, z-gradient, and echo-antiecho sensitivity enhancement (Palmer et al., 1991; Kay et al., 1992; Schleucher et al., 1994)
↵ c 1H, 1H-COSY: homonuclear correlated spectroscopy. Magnitude experiment with z-gradient (Hurd, 1990); von Kienlin et al., 1991)
↵ d Long-range 1H, 13C-COSY, HMBC experiment: heteronuclear correlated spectroscopy. Heteronuclear multiple bond correlation experiment with 1H detection and z-gradient (Bax et al., 1986; Willker et al., 1993)