Compound 16: isolated in 86% yield as a white solid; mp: 111.9ꢀ-113.2ꢀ; 1H NMR (400 MHz, CDCl ) δ 5.57 (m, 2H), 4.85 (s, 1H),
ACCEPTED MANUSCRIPT
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4.68 (s, 1H), 4.04 (s, 4H, 2CH2), 3.01 (s, 1H), 2.94 (s, 1H), 2.29-2.21 (m, 2H), 2.13-1.93 (m, 4H), 1.88-1.78 (m, 2H), 1.75 (s, 3H), 1.70 (m,
1H), 1.62-1.52 (m, 4H), 1.46-1.24 (m, 7H), 1.16-1.02 (m, 3H), 0.97 (m, 1H), 0.91 (d, J = 6.6 Hz, 3H), 0.89 (s, 3H), 0.84-0.77 (m, 2H), 0.65 (s,
3H); 13C NMR (100 MHz, CDCl3) δ 173.23 (2C), 148.40, 113.33, 79.82 (2C), 71.71 (2C), 56.85, 56.09, 51.25, 48.46, 42.59, 40.06, 38.69,
35.59, 35.30, 33.47, 33.37, 32.25, 31.68, 30.03, 29.37, 29.33, 28.31, 27.86, 24.34, 23.52, 21.11, 18.51, 17.71, 12.15; HRMS (ESI): calcd for
C32H48N2NaO2 [M+Na]+ 515.3613, found [M+Na]+ 515.3635.
Compound 17: isolated in 88% yield as a white solid; mp: 203.8ꢀ-205.1ꢀ; 1H NMR (400 MHz, CDCl3) δ 8.25 (s, 2H), 7.71 (d, J = 4.6
Hz, 2H), 6.83-6.22 (m, 2H), 4.83 (s, 1H), 4.70 (s, 1H), 3.25-2.87 (m, 4H), 2.15 (m, 1H), 1.95-1.81 (m, 5H), 1.74 (s, 3H), 1.67-1.58 (m, 4H),
1.52-1.41 (m, 4H), 1.36-1.25 (m, 3H), 1.20-1.11 (m, 3H), 0.98 (d, J = 6.0 Hz, 3H), 0.93 (s, 3H), 0.90-0.82 (m, 2H), 0.67 (s, 3H); 13C NMR
(100 MHz, CDCl3 /CD3OD) δ 173.41 (2C), 148.09, 144.41 (2C), 128.68 (2C), 113.58, 109.94 (2C), 56.95, 56.19, 51.19, 48.57, 42.80, 40.16,
38.98, 35.72, 35.61, 32.38, 32.08, 31.20, 30.75, 28.41, 28.13, 27.90, 24.52, 23.71, 21.36, 18.62, 17.76, 12.21; HRMS (ESI): calcd for
C32H46N4NaO2 [M+Na]+ 541.3518, found [M+Na]+ 541.3540.
Compound 18: isolated in 90% yield as a white solid; mp: 119.6ꢀ-120.7ꢀ; 1H NMR (400 MHz, CDCl3) δ 4.79 (s, 1H), 4.65 (s, 1H),
3.69-3.41 (m, 8H), 2.43-2.32 (m, 10H), 2.29 (s, 6H), 2.22-2.07 (m, 2H), 2.03-1.91 (m, 2H), 1.82 (m, 1H), 1.71 (s, 3H), 1.70-1.65 (m, 2H),
1.59-1.53 (m, 3H), 1.42-1.23 (m, 8H), 1.14-0.96 (m, 4H), 0.90 (d, J = 6.4 Hz, 3H), 0.88 (s, 3H), 0.85-0.79 (m, 2H), 0.63 (s, 3H); 13C NMR
(100 MHz, CDCl3) δ 172.19, 172.17, 148.38, 113.19, 56.81, 56.10, 55.35, 55.28, 54.81 (2C), 51.51, 48.59, 46.08, 46.06, 45.56 (2C), 42.55,
41.50, 41.44, 40.01, 38.85, 35.75, 35.27, 33.15, 32.23, 31.52, 30.38, 28.30, 27.97, 26.49, 24.32, 23.36, 21.12, 18.59, 17.76, 12.09; HRMS
(ESI): calcd for C36H63N4O2 [M+H]+ 583.4951, found [M+H]+ 583.4930.
Compound 19: isolated in 95% yield as a white solid; mp: 156.4ꢀ-157.6ꢀ; 1H NMR (400 MHz, CDCl3) δ 4.82 (s, 1H), 4.68 (s, 1H),
3.47-3.39 (m, 8H), 2.35-2.26 (m, 2H), 2.19-2.08 (m, 2H), 2.03 (m, 1H), 1.99-1.92 (m, 5H), 1.88-1.81 (m, 5H), 1.75 (s, 3H), 1.70 (m, 2H),
1.65-1.55 (m, 3H), 1.45-1.25 (m, 8H), 1.17-0.98 (m, 4H), 0.92 (d, J = 6.4 Hz, 3H), 0.90 (s, 3H), 0.87-0.81 (m, 2H), 0.66 (s, 3H). 13C NMR
(100 MHz, CDCl3) δ 172.40, 172.27, 148.34, 113.16, 56.92, 56.28, 51.37, 48.64, 46.77, 46.74, 45.81, 45.76, 42.60, 40.14, 38.70, 35.81, 35.32,
32.61, 32.35, 31.99, 31.11, 28.33, 28.07, 28.03, 26.30 (2C), 24.56, 24.54, 24.39, 23.70, 21.13, 18.64, 17.74, 12.15; HRMS (ESI): calcd for
C34H56N2NaO2 [M+Na]+ 547.4239, found [M+Na]+ 547.4261.
Compound 20: isolated in 86% yield as a white solid; mp: 139.6ꢀ-140.4ꢀ; 1H NMR (400 MHz, CDCl3) δ 4.80 (s, 1H), 4.66 (s, 1H),
3.65 (m, 8H), 3.61 (m, 4H), 3.45 (m, 4H), 2.49-2.29 (m, 2H), 2.24-2.09 (m, 2H), 1.99 (m, 2H), 1.83-1.74 (m, 5H), 1.73 (s, 3H), 1.62-1.55 (m,
3H), 1.45-1.23 (m, 7H), 1.16-1.05 (m, 3H), 0.93 (d, J = 6.4 Hz, 3H), 0.90 (s, 3H), 0.87-0.81 (m, 2H), 0.65 (s, 3H); 13C NMR (100 MHz, CDCl3)
δ 172.48, 172.46, 148.41, 113.23, 67.10, 67.05, 66.83, 66.78, 56.82, 56.12, 52.11, 51.61, 48.62, 46.20, 42.56, 42.08, 42.00, 40.03, 38.86, 35.75,
35.28, 33.09, 32.24, 31.44, 30.24, 28.31, 27.95, 26.39, 24.33, 23.29, 21.14, 18.59, 17.78, 12.10; HRMS (ESI): calcd for C34H57N2O4 [M+H]+
557.4318, found [M+H]+ 557.4342.
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Compound 21: isolated in 88% yield as white solid; H NMR (400 MHz, CDCl3) δ 4.80 (s, 1H), 4.66 (s, 1H), 3.67-3.53 (m, 4H),
3.51-3.21 (m, 12H), 2.42-2.31 (m, 2H), 2.25-2.09 (m, 2H), 2.05-1.93 (m, 2H), 1.90-1.78 (m, 2H), 1.72 (s, 3H), 1.68 (m, 1H), 1.63-1.53 (m,
3H), 1.46 (s, 18H), 1.43-1.23 (m, 8H), 1.18-0.97 (m, 4H), 0.92 (d, J = 6.4 Hz, 3H), 0.90 (s, 3H), 0.87-0.80 (m, 2H), 0.64 (s, 3H).
Compound 22: isolated in 89% yield as a white solid; mp: 125.5ꢀ-126.4ꢀ; 1H NMR (400 MHz, CDCl3) δ 4.78 (s, 1H), 4.64 (s, 1H),
3.70-3.38 (m, 8H), 2.51-2.28 (m, 14H), 2.21-2.07 (m, 2H), 2.03-1.90 (m, 2H), 1.82 (m, 1H), 1.70 (s, 3H), 1.68-1.62 (m, 2H), 1.58-1.50 (m,
3H), 1.42-1.21 (m, 8H), 1.12 (m, 1H), 1.06 (t, J = 7.2 Hz, 6H), 0.97 (m, 1H), 0.89 (d, J = 6.4 Hz, 3H), 0.87 (s, 3H), 0.84-0.78 (m, 4H), 0.61 (s,
3H); 13C NMR (100 MHz, CDCl3) δ 172.03, 172.00, 148.23, 113.10, 56.70, 55.98, 53.11, 53.05, 52.47, 52.23, 51.34, 48.47, 45.61, 42.44,
41.52, 41.45, 39.91, 38.74, 35.65, 35.17, 33.05, 32.13, 31.43, 30.27, 29.43, 28.20, 27.87, 26.89, 26.37, 25.42, 24.23, 23.32, 22.81, 21.02, 18.49,
17.66, 12.00, 11.92; HRMS (ESI): calcd for C38H67N4O2 [M+H]+ 611.5264, found [M+H]+ 611.5289.
Compound 23: isolated in 87% yield as a white solid; mp: 128.6ꢀ-129.7ꢀ; 1H NMR (400 MHz, CDCl3) δ 4.82 (s, 1H), 4.68 (s, 1H),
3.70-3.56 (m, 4H), 3.54-3.39 (m, 4H), 2.77-2.65 (m, 2H), 2.55-2.43 (m, 8H), 2.42-2.31 (m, 2H), 2.25-2.11 (m, 2H), 2.07-1.94 (m, 2H), 1.74 (s,
3H), 1.72-1.69 (m, 5H), 1.63-1.55 (m, 3H), 1.45-1.26 (m, 7H), 1.17-1.09 (m, 3H), 1.05 (d, J = 6.4 Hz, 12H), 0.93 (d, J = 6.3 Hz, 3H), 0.91 (s,
3H), 0.87-0.82 (m, 2H), 0.65 (s, 3H); 13C NMR (100 MHz, CDCl3) δ 172.14 (2C), 148.42, 113.21, 56.85, 56.13, 54.67, 51.49, 49.14, 49.09,
48.62, 48.49, 48.46, 46.08, 42.58, 41.96, 41.89, 40.06, 38.90, 35.80, 35.32, 33.18, 32.29, 31.59, 30.42, 29.56, 29.18, 28.35, 28.02, 26.49, 24.36,
23.46, 21.17, 18.63, 18.49 (4C), 17.79, 12.13; HRMS (ESI): calcd for C40H71N4O2 [M+H]+ 639.5577, found [M+H]+ 639.5606.