23-hydroxybetulinic acid 3-site modified derivative, and preparation method and application thereof
A derivative, betulinic acid technology, applied in the field of preparation, 3-position modified derivatives of 23-hydroxy betulinic acid, can solve rare problems
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Embodiment 1
[0047]
[0048] 3-Pyridylamide-23-acetyl-lupine-20(29)-en-28-oic acid benzyl ester
[0049] 23-HBA (10.0g, 21.0mmol) was dissolved in DMF (120mL), and potassium carbonate (10.0g, 72mmol) and benzyl bromide (3mL, 25.0mmol) were gradually added thereto. After reacting at room temperature for 2h, 2 Double the volume of water (240mL), the product precipitated, and the crude product was obtained by suction filtration (it can be directly injected into the next step), and column chromatography (petroleum ether: ethyl acetate = 2:1-1:1) gave a white solid 28-benzyl protected 23-HBA Derivatives 1.
[0050] Compound 1 (1.00g, 2.05mmol) was dissolved in dichloromethane (40mL), DMAP (0.052g, 0.41mmol) was added, acetic anhydride (211.7μL, 2.26mmol) was added dropwise under stirring, and the reaction was monitored at room temperature to The raw materials disappeared, the reaction solution was concentrated, extracted with ethyl acetate (50mL×3), the organic layers were combined, washed ...
Embodiment 2
[0054]
[0055] 3-Pyrazinamide-23-acetyl-lupine-20(29)-en-28-oic acid benzyl ester
[0056] The synthetic method refers to the synthesis of Example 1, 48.9%. 1 H NMR (500MHz, Chloroform-d) δ9.34(d, J=3.8Hz, 1H), 8.74(q, J=2.6Hz, 2H), 7.37-7.29(m, 5H), 5.16-5.01(m, 2H), 4.72(d, J=2.4Hz, 1H), 4.60(s, 1H), 4.25-4.11(m, 2H), 3.97(dd, J=16.3, 11.5Hz, 1H), 3.01(td, J =10.8, 4.7Hz, 1H), 2.30-2.12(m, 2H), 2.08-1.99(m, 1H), 1.95(d, J=4.2Hz, 3H), 1.93-1.81(m, 3H), 1.76- 1.68(m, 3H), 1.64-1.53(m, 2H), 1.43(d, J=8.0Hz, 2H), 1.42-1.39(m, 2H), 1.38(d, J=6.4Hz, 2H), 1.35 -1.32(m, 2H), 1.29(d, J=4.9Hz, 2H), 1.27-1.24(m, 2H), 1.04(ddd, J=17.4, 8.0, 4.4Hz, 3H), 0.96(d, J =17.7Hz, 2H), 0.92(d, J=4.8Hz, 1H), 0.89(d, J=2.8Hz, 3H), 0.86(s, 3H), 0.83(s, 1H), 0.77(s, 3H ). 13 C NMR (125MHz, Chloroform-d) δ175.8, 169.6, 163.7, 150.5, 147.3, 146.2, 144.7, 143.9, 136.5, 128.5, 128.2, 128.0, 109.7, 67.9, 65.7, 56.5, 51.0, 50.9, 49.4, 49 ESI-MS m / z: 710.5 [M+H] + ; HR-MS (ESI) m / z: calculated ...
Embodiment 3
[0058]
[0059] 3-Cyclohexaneamide-23-acetyl-lupine-20(29)-en-28-oic acid benzyl ester
[0060] The synthetic method refers to the synthesis of Example 1, 45.7%. 1 H NMR (300MHz, Chloroform-d) δ7.37-7.32(m, 5H), 5.17-5.08(m, 3H), 4.72(s, 1H), 4.60(s, 1H), 4.09-4.01(m, 2H ), 3.90(d, J=11.4Hz, 1H), 3.47(d, J=11.5Hz, 1H), 3.05-2.99(m, 1H), 2.40-2.26(m, 2H), 2.19(t, J= 10.6Hz, 1H), 1.95(s, 3H), 1.68(s, 3H), 0.93(s, 3H), 0.82(s, 3H), 0.75(s, 3H), 0.70(s, 3H); ESI- MS m / z: 714.5[M+H] + ; HR-MS (ESI) m / z: calculated for C 46 h 68 NO 5 [M+H] + :714.5092, found: 714.5089.
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