. Author manuscript; available in PMC: 2019 Aug 15.

Published in final edited form as: Bioorg Med Chem. 2018 Jul 17;26(15):4452–4460. doi: 10.1016/j.bmc.2018.07.025

Table 1.

¹H and ¹³C NMR spectroscopic data of 2 and 3^a

position	2^b	2^c	3^d	3^e
1	39.19 CH₂	α 0.97 m	39.62 CH₂	α 0.91 m
		β 1.68 m		β 1.74 m
2	27.57 CH₂	1.63 m	28.25 CH2	1.54 m
		1.59 m		1.57 m
3	79.11 CH	α 3.21 m	78.54 CH	α 3.06 m
4	39.14 C		39.58 C
5	56.14 CH	α 0.74 m	56.55 CH	α 0.65 dd
				(11.6, 1.6)
6	18.42 CH₂	α 1.53 m	19.04 CH₂	α 1.49 m
		β 1.44 m		β 1.37 m
7	35.37 CH₂	α 1.28 m	38.44 CH₂	α 1.52m
		β 1.51 m		β 1.61 m
8	40.52 C		41.07 C
9	50.77 CH	α 1.33 m	52.04 CH	α 1.51 m
10	37.28 C		38.20 C
11	21.67 CH₂	β 1. 23 m	21.42 CH₂	1.48 m
		α 1. 49 m		1.32 m
12	24.99 CH2	α 1.47 m	26.91 CH2	α 2.14 m
		β 1. 70 m		β 1. 67 m
13	42.55 CH	β 1.62 m	40.49 CH	β 2.35 m
14	50.48 C		59.95 C
15	31.33 CH2	α 1. 07 m	28.36 CH2	α 1.51 m
		β 1.46 m		β 1.27 m
16	27.57 CH₂	1.63 m	34.99 CH2	α 2.32 m
		1.59 m		β 1.45 m
17	50.27 CH	α 1. 76 m	56.96 C
18	15.63 CH3	β 0.96 s	52.64 CH	α 1. 70 m
19	16.37 CH₃	β 0.84 s	47.91 CH	β 3.09 m
20	75.33 C		150.95 C
21	25.54 CH₃	β 1.15 s	31.06 CH₂	β 1. 87 m
				α 1.39 m
22	36.19 CH₂	1.46 m	37.56 CH₂	β 1. 41 m
		1.27 m		α 1.91 m
23	29.52 CH₂	1.26 m	28.62 CH₃	α 0. 93 s
24	76.13 CH	4.08 t (5.6)	16.19 CH₃	β 0.74 s
25	147.91 C		17.09 CH₃	β 0.88 s
26	110.93 CH	4.85 br s	17.42 CH₃	β 1.02 s
		4.97 br s
27	18.17 CH₃	1.73 s	177.05 C
28	28.15 CH₃	α 0.97 s	176.84 C
29	15.51 CH3	β 0.77 s	110.50 CH₂	4.59 br s
				4.73 br s
30	16.63 CH3	α 0.88 s	19.11 CH3	1.69 s
OH-3		β 3.67 brs		3.35 brs
OCH₃−28			51.67 CH₃	3.67 s

Assignments of chemical shifts are based on the analysis of 1D- and 2D-NMR spectra. The overlapped signals were assigned from ¹H −¹H COSY, HSQC, and HMBC spectra without designating multiplicity.

¹³C NMR spectroscopic data (δ) measured in CDCl₃ at 100.61 MHz and referenced to the solvent residual peak at δ 77.16.⁴⁰

¹H NMR spectroscopic data (δ) measured in CDCl₃ at 400.13 MHz and referenced to the solvent residual peak at δ 7.26.₄₀

¹³C NMR spectroscopic data (δ) measured in acetone-d₆ (different from that used in literature²⁰) at 100.61 MHz and referenced to the solvent residual peak at δ 29.84.⁴⁰

¹H NMR spectroscopic data (δ) measured in acetone-d₆ (different from that used in hat used in literature²⁰) at 400.13 MHz and referenced to the solvent residual peak at δ 2.05.⁴⁰