Table 2.
1H NMR Chemical Shifts of Compounds 3–6a
position | 3 | 4 | 5 | 6 |
---|---|---|---|---|
1 | 1.48b | 1.62b | 1.63b | 3.88, m |
1.95, m | 1.82b | 1.82b | ||
2 | 2.46b | 2.65, td (14.0, 4.6) | 2.67, td (14.0, 4.5) | Hα, 2.72, dd (6.1, 17.3) |
2.50, ddd (14.2, 5.7, 3.5) | 2.52, ddd (14.2, 5.7, 3.5) | Hβ, 2.72, dd (12.1, 17.3) | ||
5 | 1.35b | 1.78b | 1.80b | |
6 | 1.50b | 1.43b | 1.44b | 6.46, s |
1.77b | 1.77b | |||
7 | 1.42b | 1.30b | 1.31b | |
8 | 2.30, m | |||
9 | 1.43b | 1.42b | 1.42b | Hα, 1.43,ddd (6.0, 5.7, 12.5) |
Hβ, 2.16, ddd (2.0, 5.0, 12.8) | ||||
11 | 1.35b | 1.55b | 1.55b | 2.46, hep (6.6) |
1.55b | 1.26b | 1.26b | ||
12 | 1.19b | 1.10b | 1.12, d (6.8) | |
2.03, brd (10.0) | 1.86b | 1.12, d (6.8) | ||
13 | 2.07, td (12.0, 3.0) | 1.75b | 1.70b | |
14 | 1.09, s | |||
15 | 1.58b | 1.10b | 1.10b | 4.45, brs |
1.20b | 1.45b | 1.45b | ||
16 | 1.60b | 1.30b | 1.30b | |
1.75b | 1.78b | 1.78b | ||
17 | 3.48, d (11.4) | 1.79b | 1.91b | |
18 | 1.07, s | 1.02, s | 1.05, s | |
19 | 0.96, s | 1.08, s | 1.10, s | |
21 | 1.15, s | 1.17, s | ||
22 | Hα1.48b | 1.71b | 1.71b | |
Hβ2.03, td (13.2, 4.8) | ||||
23 | Hβ 1.56b | 1.80b | 1.88b | |
Hα 1.73b | 1.82b | |||
24 | 3.26, d (12.0) | 3.77, t (7.2) | 3.65, dd (9.9, 5.6) | |
26 | 1.16, s | 1.20, s | 1.21, s | |
27 | 1.20, s | 1.10, s | 1.13, s | |
28 | 1.08, s | 1.48, s | 1.50, s | |
29 | 1.03, s | 1.40, s | 1.42, s | |
30 | 0.98, s | 0.86, s | 0.88, s |
Measured at 600 MHz and obtained in CDCl3 with TMS as internal standard; J values (Hz) are given in parentheses. Assignments supported with 1H-1H COSY, HSQC, and HMBC spectra.
Multiplicity patterns unclear due to signal overlapping.