Table 3.

NMR data for TFA salt of hemiasterlin D (4) recorded in DMSO-d₆ ^a at 30 °C.

Position	δCb	δH (J in Hz)	gCOSY	ROESY	gHMBCAD
2	125.2	7.20, s		22, 27	3, 4, 9, 10, 27
3	118.0
4	125.4
5	120.2	8.11, d (7.2)	6	11, 22	7, 9
6	119.0	7.11, t (7.2, 7.8)	5, 7		4, 8
7	121.2	7.15, t (7.2, 7.8)	6, 8		5, 9
8	110.8	7.54, d (8.4)	7	27	4, 6
9	136.5
10	37.6
11	66.9	4.47, d (10.2)	NH	5, 13, 21, 22
12	165.9
13		8.90, d (7.8)	14	11, 23	12
14	55.4	4.87, d (7.8)	13	24, 23	12, 14a, 15, 23
14a	34.5
15	169.9
17	56.0	4.93, t (9.6, 10.2)	17a, 18	25, 25′, 26	17a, 18, 19
17a	28.6	2.03, m	17, 25, 25′	18, 24
18	138.0	6.68, d (9.6)	17	24, 17a, 25	20, 26
19	131.7
20	168.4
21	33.3	2.24, t (4.2)	NH	11, 23	11
22	26.9	1.37, s		5, 11	3, 10, 11, 22′
22′	21.9	1.38, s		2	3, 10, 11, 22
23	26.1	1.01 (s)		14, 24	14, 14a
24	31.0	3.04 (s)		14, 17a, 18, 23	15, 17
25	19.0	0.82, d (6.0)			17, 17a, 25′
25′	19.0	0.81, d (6.0)			17, 17a, 25
26	13.3	1.80, s		17	18, 19, 20
27	76.3	6.34, s		2, 8, 29	2, 9, 28
28	167.6
29		8.10, d (8.4)	30	27, 37	28
30	53.9	4.73, d (9.0)	29	37, 38	28, 30a, 31, 37
30a	34.8
31	170.3
33	55.5	5.01, t (9.6, 10.2)	33a, 34	39, 39′, 40	31, 33a, 34, 35, 38
33a	28.5	1.97, m	33, 39, 39′	34, 38
34	137.8	6.64, d (9.6)	33	33a, 38	36, 40
35	132.2
36	168.3
37	25.8	0.88, s		29, 30, 38, 40	30, 30a
38	30.4	2.94, s		30, 33a, 34, 37	31, 33
39	18.7	0.79, d (6.6)			33, 33a, 39′
39′	18.7	0.74, d (6.6)			33, 33a, 39
40	13.3	1.80, s		33	34, 35, 36
11-NH		8.88, brs 7.51, brs	11, 21 21
20-OH/36-OH		12.4, brs

^{a 1}H NMR at 600 MHz referenced to residual DMSO solvent (δ_H 2.50 ppm) and ¹³C NMR at 150 MHz referenced to residual DMSO solvent (δ_C 39.52 ppm); ^{b 13}C chemical shifts obtained from correlations observed in gHSQCAD and gHMBCAD spectra.