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23. C1–C7 fragment 11. 1H NMR (400 MHz, CDCl3) d 7.38–7.18 (m, 15H), 3.94–3.92
(m, 1H), 3.57–3.54 (m, 2H), 3.10–3.05 (m, 1H), 2.87–2.81 (m, 1H), 2.47–2.29
(m, 2H), 2.12–2.09 (m, 1H), 1.85–1.78 (m, 1H), 1.55–1.37 (m, 2H), 0.94 (s, 3H),
0.88–0.87 (m, 21H), 0.08–0.06 (m, 12H). 13C NMR (100 MHz, CDCl3) d 214.7,
144.3, 128.8, 128.5, 127.9, 127.0, 87.2, 73.9, 60.3, 59.9, 55.5, 37.5, 37.3, 32.4,
26.3, 26.1, 18.6, 18.4, 14.8, 7.6, ꢀ3.5, ꢀ3.6, ꢀ5.1. HRMS m/z calcld for
C41H66NO4Si2 (M+NH4) 692.4530, found 692.4538. ½a D22:5
ꢀ 17:5 (c 2.55, CHCl3).
ꢁ
24. Photoaffinity analog 3: 1H NMR (400 MHz, CDCl3) d 7.75 (dm, J = 7.9 Hz, 1H),
7.64 (t, J = 1.7 Hz, 1H), 7.39 (t, J = 7.9 Hz, 1H), 7.18 (dm, J = 8 Hz, 1H), 6.98 (s,
1H), 6.58 (s, 1H), 5.38 (m, 2H), 5.34 (d, J = 9.9 Hz, 1H), 4.37 (m, 2H), 4.20 (ddd,
J = 11.2 Hz, J = 9.5 Hz, 5.7 Hz, 1H), 3.73 (d, J = 4.4 Hz, 1H), 3.45 (br s, 1H), 3.18
(qd, J = 6.7 Hz, J = 1.1 Hz, 1H), 3.16 (s, 1H), 2.67 (m + s, 4H), 2.57 (dd, J = 14.9 Hz,
J = 11.5 Hz, 1H), 2.41 (dd, J = 14.9 Hz, 2.4 Hz, 1H), 2.35 (m, 1H), 2.28 (m, 1H),
2.16 (m, 2H), 2.08 (s, 3H), 1.54–1.8 (m, 4H), 1.23 (t, J = 7.2 Hz, 2H), 1.21 (d,
J = 6.9 Hz, 3H), 1.16 (s, 3H), 1.00 (d, J = 7.1 Hz, 3H). 13C NMR (125 MHz, CDCl3)
219.7, 170.2, 165.5, 165.1, 151.9, 140.7, 138.6, 133.4, 131.7, 129.9, 126.0, 125.2,
123.6, 119.9, 119.5, 115.9, 78.4, 73.9, 71.9, 61.9, 56.2, 41.6, 38.9, 38.6, 33.5,
32.5, 31.8, 30.7, 19.1, 15.9, 15.2, 14.2, 13.7, 13.1. IR (neat) mmax 3515, 2358,
2115, 1724 cmꢀ1. HRMS m/z calcd for C34H44N4O7S (M+H) 653.3009, found
653.2990. ½a 2D6
ꢀ 51:6 (c 0.480, CHCl3).
ꢁ
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