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J = 6.4 Hz, 3H, H-600), 1.06 (d, J = 6.4 Hz, 3H), 1.02 (s,
9.6 Hz, 1H, H-30), 5.68 (s, 1H, H-10), 5.60 (t, J = 10.0 Hz,
1H, H-40), 5.46 (s, 1H, PhCH), 4.93 (m, 1H, H-50), 4.65 (d,
J = 9.6 Hz, 1H, H-1), 4.36 (dd, J = 4.4, 10.8 Hz, 1H, H-
6a), 4.10 (t, J = 8.0 Hz, 1H), 3.83 (t, J = 8.0 Hz, 1 H), 3.73
(t, J = 10.0 Hz, 1H), 3.55–3.44 (m, 2H), 2.87–2.80 (m, 2H),
1.40–1.30 (m, 6H, SCH2CH3, H-60), 0.65 (br s, 9H, CMe3),
ꢀ0.01 (2s, 6H, SiMe2). ESI-MS: 910.2 (M+Na)+.
(m, 40H, OBz), 6.70 (dd, J = 2.4, 10.4 Hz, 1H, H-300), 6.51
(br s, 1H, H-200), 6.37 (d, J = 8.4 Hz, 1H, H-1000), 6.30 (t,
J = 10.0 Hz, 1H, H-400), 6.13 (t, J = 9.2, 8.8 Hz, 1H), 5.99
(t, J = 9.6 Hz, 1H), 5.78 (t, J = 9.6 Hz, 1H), 5.72 (br s, 1H,
H-100), 5.64 (d, J = 3.6 Hz, 1H, H-10), 5.35 (dd, J = 9.2,
9.6 Hz, 1H), 5.29 (br s, 1H, H-6), 4.96–4.87 (m, 10H),
4.82–4.75 (m, 2H), 4.70–4.59 (m, 3H), 4.37–4.34 (dd,
J = 3.6, 9.6 Hz, 1H), 4.12–4.08 (dd, J = 6.4, 10.8 Hz, 1H),
4.09–3.96 (dd, J = 6.4, 10.8 Hz, 1H), 3.87 (m, 1H), 2.92
(m, 1H), 2.77 (m, 1H), 2.29–2.24 (m, 2H), 2.00 (s, 3H,
COCH3), 1.59 (d, J = 7.0 Hz, 3H), 1.34 (d,J = 6.8 Hz, 3H,
H-600), 1.09 (s, 3H), 0.95 (s, 3H), 0.92 (d, J = 6.4 Hz, 3H).
13C NMR (400 MHz, CDCl3): 169.60, 165.48, 165.15,
164.99, 164.91, 164.68, 164.57, 164.33, 139.13, 133.65,
133.36, 109.31, 99.41, 98.58, 96.05, 80.84, 79.98, 79.01,
74.43, 72.20, 71.01, 70.68, 70.42, 70.14, 68.19, 67.35, 62.60,
55.45, 49.06, 39.68, 39.50, 38.77, 35.83, 32.13, 31.31, 30.50,
29.30, 27.75, 27.05, 19.98, 19.56, 18.29, 17.04, 15.86, 15.32,
15.21. ESI-MS:1905 (M+Na+1)+(base).
3H), 0.96 (d, J = 6.8 Hz, 3H), 0.92–0.84 (m, 6H), 0.79 (s,
3H). 13C NMR (75 MHz, CDCl3): 217.90, 213.29, 171.27,
170.98, 170.69, 170.15 (2· C), 169.84, 140.38, 121.35,
99.64, 97.37, 79.21, 76.30, 71.51, 71.34, 71.14, 69.54, 69.16,
69.00, 66.32, 66.13, 62.43, 51.17, 49.67, 43.32, 41.63, 39.67,
38.54, 38.44, 37.15, 36.78, 2.04, 31.55, 30.89, 29.52, 26.67,
22.77, 20.94, 20.89, 20.79, 20.50, 20.12, 19.14, 17.21, 16.78,
15.35, 14.37, 14.08, 12.96, 11.36. ESI-MS: 1014.6
(M+Na)+.
1
Compound 21: H NMR (400 MHz, CDCl3), d 8.70–6.88
Compound 7 1H NMR (400 MHz, CDCl3), d 8.01–7.30
(m, 20H, OBz), 6.04 (t, J = 9.6 Hz, 1H, 1H, H-3000), 5.71
(dd, J = 9.9, 9.6 Hz, 1H, H-4000), 5.44–5.36 (m, 3H, H-6, H-
100, H-200), 5.33–5.29 (dd, J = 3.3, 10.5 Hz, 1H, H-300),
5.16–5.04 (m, 2H, H-1000, H-2000), 4.86 (t, J = 9.9, 9.3 Hz,
1H, H-400), 4.66–4.61 (dd, J = 3.0, 12.3 Hz, 1H, H-6a000),
4.56–4.50 (dd, J = 4.8, 12.3 Hz, 1H, H-6b000), 4.43–4.38 (m,
2H, H-10, H-500), 4.25–4.19 (m, 1H), 4.17–4.00 (m, 2H),
3.69 (t, J = 8.0 Hz, 1H), 3.48–3.33 (m, 3H), 2.18 (s, 3H,
OAc), 2.08 (s, 3H, OAc), 2.05 (s, 3H, OAc), 2.02 (s, 3H,
OAc), 2.03 (s, 3H, OAc), 1.90 (s, 3H, OAc), 1.23 (s, 3H),
1.08 (d, J = 6.0 Hz, 3H, H-600), 1.01 (s, 3H), 0.97 (d,
J = 6.6 Hz, 3H), 0.79 (d, J = 2.4 Hz, 3H), 0.78 (s, 3H). 13
C
NMR (75 MHz, CDCl3): 170.84, 170.68, 170.17, 169.95,
169.34, 166.08, 165.44, 165.15, 165.09, 140.19, 133.32,
133.19, 132.99, 129.89, 129.79, 129.70, 129.60, 129.24,
129.08, 128.84, 128.44, 128.33, 128.19, 128.12, 121.96,
109.28, 99.22 (2· C), 96.58, 80.76, 80.23, 78.73, 76.10,
72.75, 72.58, 72.17, 71.32, 71.07, 69.87, 66.76, 68.81, 68.15,
66.83, 66.54, 62.94, 62.43, 62.06, 56.44, 50.02, 41.59, 40.24,
39.70, 38.27, 37.11, 36.87, 32.07, 31.82, 31.39, 30.27, 29.67,
29.46, 28.78, 20.81, 20.75, 20.67, 19.26, 17.12, 16.27, 14.50.
ESI-MS: 1595.8(M+Na)+.
Compound 2: 13C NMR (100 MHz, pyridine-d5): 140.71,
121.77, 109.22, 105.20, 101.79, 99.91, 81.94, 81.06,
78.46, 78.24, 78.04, 77.70, 77.25, 76.18, 74.93, 74.07,
72.72, 72.43, 71.14, 69.46, 66.82, 62.84, 62.01, 61.83,
56.58, 50.22, 41.92, 40.41, 39.80, 38.87, 37.44, 37.08,
32.26, 32.19, 31.79, 31.64, 30.57, 30.10, 29.96, 29.23,
21.06, 19.36, 18.64, 17.31, 16.31, 15.03. ESI-MS: 907
(M+NaꢀMeOH)+.
1
Compound 16: H NMR (400 MHz, CDCl3), d 8.07–7.23
(m, 20H, OBz), 5.81 (br s, 1H, H-20), 5.78 (dd, J = 3.2,