Table 4.

¹³C and ¹H NMR chemical shifts and HMBC and ROESY correlations of the aglycone moiety of chitonoidoside K (3).

Position	δC Mult. a	δH Mult. (J in Hz) b	HMBC	ROESY
1	36.0 CH2	1.30 m (α)		H-3, H-5, H-11, H-19
2	26.9 CH2	1.95 m (β)
		1.76 m
3	88.9 CH	3.14 dd (3.3; 11.8)		H-1, H-5, H-31, H1-Xyl1
4	39.2 C
5	48.0 CH	0.88 m	C: 10, 19, 30	H-3, H-31
6	22.9 CH2	1.89 m		H-31
7	119.8 CH	5.64 m		H-15, H-32
8	146.7 C
9	47.3 CH	3.32 brd (14.1)		H-19
10	35.4 C
11	22.7 CH2	1.65 m (α)		H-1
		1.42 m (β)		H-19
12	30.2 CH2	1.95 m
13	58.7 C
14	51.2 C
15	34.1 CH2	1.73 m (β)		H-7, H-32
		1.49 d (13.1) (α)		H-32
16	24.4 CH2	1.93 m (β)
		1.72 m (α)		H-32
17	53.0 CH	2.17 t (12.3)		H-21, H-32
18	180.9 C
19	23.9 CH3	1.08 s	C: 5, 9, 10	H-2, H-9
20	84.7 C
21	25.9 CH3	1.38 s	C: 17, 20, 22	H-12, H-17, H-24
22	39.2 CH2	1.64 m
		1.54 m
23	21.8 CH2	1.31 m
		1.23 m
24	37.8 CH2	1.88 m	C: 25
25	145.3 C
26	110.7 CH2	4.70 brs	C: 24, 27	H-27
		4.66 brs	C: 24, 27	H-24
27	22.0 CH3	1.61 s	C: 24, 25, 26	H-24, H-26
30	17.1 CH3	0.89 s	C: 3, 4, 5, 31	H-31
31	28.5 CH3	1.09 s	C: 3, 4, 5, 30	H-3, H-5, H-6, H-30, H-1 Xyl1
32	30.8 CH3	1.08 s	C: 8, 13, 14, 15	H-7, H-12, H-17

^a Recorded at 125.67 MHz in C₅D₅N/D₂O (4/1). ^b Recorded at 500.12 MHz in C₅D₅N/D₂O (4/1). The original spectra of 3 are provided as Figures S17–S22.