3-position modified derivative of 23-hydroxybetulinic acid, preparation method and application
A derivative, betulinic acid technology, applied in the field of 23-hydroxybetulinic acid 3-modified derivatives, preparation field, can solve rare problems
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Embodiment 1
[0047]
[0048] 3-Pyridylamide-23-acetyl-lupin-20(29)-ene-28-acid benzyl ester
[0049] 23-HBA (10.0 g, 21.0 mmol) was dissolved in DMF (120 mL), potassium carbonate (10.0 g, 72 mmol) and benzyl bromide (3 mL, 25.0 mmol) were gradually added to it, and 2 h was added after the reaction at room temperature for 2 h. twice the volume of water (240 mL), the product was precipitated, and the crude product was obtained by suction filtration (which can be directly added to the next step). 23-HBA derivative 1.
[0050] Compound 1 (1.00 g, 2.05 mmol) was dissolved in dichloromethane (40 mL), DMAP (0.052 g, 0.41 mmol) was added, acetic anhydride (211.7 μL, 2.26 mmol) was added dropwise under stirring, and the reaction was monitored at room temperature until The raw materials disappeared, the reaction solution was concentrated, extracted with ethyl acetate (50 mL×3), the organic layers were combined, washed three times with water, washed with saturated sodium chloride, dried over anhy...
Embodiment 2
[0054]
[0055] 3-Pyrazinamide-23-acetyl-lupin-20(29)-ene-28-acid benzyl ester
[0056] The synthesis method refers to the synthesis of Example 1, 48.9%. 1 H NMR (500MHz, Chloroform-d) δ 9.34 (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: cal...
Embodiment 3
[0058]
[0059] 3-Cyclohexaneamide-23-acetyl-lupin-20(29)-ene-28-acid benzyl ester
[0060] The synthesis method refers to the synthesis of Example 1, 45.7%. 1 H NMR (300MHz, Chloroform-d) δ 7.37-7.32 (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); 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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