CA-4 derivatives and preparation method and medicinal application thereof
A use and drug technology, applied in the field of Combretastatin A-4 derivatives, in the field of tumor blood vessel inhibitory effect, can solve the problems of affecting the clinical use effect, easy to produce drug resistance, etc.
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Embodiment 1
[0089] N-(2,3,4,6-tetra-O-acetyl-1-deoxy-β-D-glucopyranosyl)-4-((Z)2'-methoxy-5'-(3 ", 4", 5 "-trimethoxystyryl) phenoxy) -4-oxobutyramide (I-2) preparation
[0090] (E)-3-(3’-Hydroxy-4’-methoxy)phenyl-2-(3”, 4”, 5”-tri-methoxy)phenyl-acrylic acid (1)
[0091] Add 3,4,5-trimethoxyphenylacetic acid (50g, 0.22mol), 3-hydroxyl-4-methoxybenzaldehyde (34g, 0.22mol), 62.5ml triethylamine and 150ml Acetic anhydride, stir and heat up to 140°C, react for 4h, stop heating, cool to 10°C, slowly add 200ml of concentrated hydrochloric acid dropwise, and leave overnight at room temperature. A khaki solid precipitated out, the reaction was stopped and the solid was filtered out, and recrystallized with about 100ml of ethanol to obtain 47.5g of a pure yellow needle, with a yield of 61%, m.p.184-186°C (literature value: 184-186°C [Bioorg . Med. Chem., 2005, 13(11): 3853-3864])
[0092] 1 HNMR (300MHz, DMSO), δ (ppm): 12.42 (1H, s, COOH), 8.95 (1H, s, OH), 7.57 (1H, s, =CH), 6.81 (1H, d, J ...
Embodiment 2
[0106] N-(2,3,4,6-tetra-O-acetyl-1-deoxy-β-D-galactopyranosyl)-4-((Z)2'-methoxy-5'-( 3 ", 4 ", 5 "-trimethoxystyryl) phenoxy) -4-oxobutyramide (I-5) preparation
[0107] Will G 2 -NH 2 (0.8g, 2.3mmol) was dissolved in DMF (12ml). Then 2b (0.92g, 2.3mmol), EDCI (0.44g, 2.3mmol), HOBt (0.31g, 2.3mmol) were added in batches successively, and stirred at room temperature for 24h. Add dichloromethane (80ml) to the reaction solution, wash with water (2×100ml), wash with saturated brine (3×100ml), dry, filter with suction, evaporate the solvent under reduced pressure, and perform silica gel column chromatography (petroleum ether / ethyl acetate=3 / 2), to obtain 1.08g of light yellow solid, yield 63.0%, m.p.85-87°C;
[0108] 1 H-NMR (300MHz, CDCl 3 ) δ (ppm): 7.12 (1H, dd, J = 8.4Hz, J = 1.8Hz, 4'-ArH), 7.01 (1H, d, J = 1.8Hz, 6'-ArH), 6.83 (1H, d , J=8.7Hz, 3'-ArH), 6.50(2H, s, 2"&6"-ArH), 6.45(2H, s, 1aH&1a'H), 6.38(1H, d, J=8.7Hz, NH) , 5.44(1H, s, H-4), 5.30~5.13(3H, m, H-1, ...
Embodiment 3
[0113] N-(1,3,4,6-tetra-O-acetyl-2-deoxy-β-D-glucopyranosyl)-4-((Z)2'-methoxy-5'-(3 ", 4", 5 "-trimethoxystyryl) phenoxy) -4-oxobutyramide (I-7) preparation
[0114] Will G 3 -NH 2 .HCl (0.77g, 2mmol) was dissolved in DMF (10ml). Dry triethylamine (0.28ml, 2mmol) was slowly added dropwise. Then 2b (0.83g, 2mmol), EDCI (0.38g, 2mmol), HOBt (0.27g, 2mmol) were added in batches successively, and stirred at room temperature for 24h. Add dichloromethane (80ml) to the reaction solution, wash with water (2×100ml), wash with saturated brine (3×100ml), dry, filter with suction, evaporate the solvent under reduced pressure, and perform silica gel column chromatography (petroleum ether / ethyl acetate=2 / 1), 0.82g of white solid was obtained, the yield was 55.0%, m.p.78-79°C;
[0115] 1 H-NMR (300MHz, CDCl 3 ) δ (ppm): 7.12 (1H, dd, J = 8.4Hz, J = 1.8Hz, 4'-ArH), 6.98 (1H, d, J = 1.8Hz, 6'-ArH), 6.82 (1H, d , J=8.4Hz, 3'-ArH), 6.49 (2H, s, 2"&6"-ArH), 6.45 (2H, s, 1aH&1a'H), 5.73~5...
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