A kind of isoandrographolide compound and its preparation method and application
A technology of ester compound and andrographis paniculata, applied in the field of isoandrographolide compounds and their preparation, can solve the problems of not being effectively contained, and achieve novel structure, good application prospects, and good antitumor activity
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Embodiment 1
[0042] The present embodiment is isoandrographolide compound 19-(2-(4-(4-aminobenzoyl) benzoate base) acetoxy) isoandrographolide (I 1 ) preparation:
[0043] (1) Add isoandrographolide (2.056g, 5.71mmol) and 100mL of dichloromethane into a 150mL round bottom flask, stir magnetically at room temperature until completely dissolved, then add potassium carbonate (1.025g, 7.42mmol). After stirring magnetically at room temperature for 30 min, bromoacetyl chloride (546 μL, 6.28 mmol) was added, and stirred magnetically at room temperature for 6 h. After the reaction was completed, the reaction solution was diluted with 100 mL of dichloromethane, washed with saturated brine (100 mL×3), dried over anhydrous magnesium sulfate, filtered, and separated by silica gel column chromatography (developing agent V 石油醚 / V 乙酸乙酯 =1 / 1), the product 19-bromoacetyl-isoandrographolide (1.330 g, 50%) was obtained as a white solid. The product identification data is: m.p.121.4°C. 1 H-NMR (CDCl 3 ,4...
Embodiment 2
[0046] The present embodiment is isoandrographolide compound 19-(3-(4-(4-aminobenzoyl) benzoate group) propionyloxy) isoandrographolide (I 2 ) preparation:
[0047] (1) Add isoandrographolide (2.043g, 5.71mmol) and 100mL of dichloromethane into a 150mL round bottom flask, stir magnetically at room temperature until completely dissolved, then add DMAP (1.047g, 7.42mmol). After magnetic stirring at room temperature for 30 min, 3-bromopropionyl chloride (627 μL, 6.28 mmol) was added and magnetic stirring at room temperature for 6 h. After the reaction was completed, the reaction solution was diluted with 100 mL of dichloromethane, washed with saturated brine (100 mL×3), dried over anhydrous magnesium sulfate, filtered, and separated by silica gel column chromatography (developing agent V 石油醚 / V 乙酸乙酯 =1 / 1), the white solid product 19-bromopropionyl-isoandrographolide (1.012 g, 37%) was obtained. The product identification data is: m.p.122.0℃. 1 H-NMR (CDCl 3,400MHz)δ:7.28(1H,...
Embodiment 3
[0050] The present embodiment is isoandrographolide compound 19-(4-(4-(4-aminobenzoyl) benzoate base) butyryloxy) isoandrographolide (I 3 ) preparation:
[0051] (1) The preparation method is the same as in Example 1, reacting isoandrographolide with 4-bromobutyryl chloride, and separating by silica gel column chromatography (developing agent V 石油醚 / V 乙酸乙酯 =1 / 1), the white solid product 19-bromobutyryl-isoandrographolide (1.553 g, 55%) was obtained. The product identification data is: m.p.122.3℃. 1 H-NMR (CDCl 3 ,400MHz)δ:7.28(1H,over signal,H-14),4.81(2H,s,H-15),4.71(1H,t,J=7.3Hz,H-12),4.45(1H,d, J=11.7Hz, H-19a), 4.16(1H, d, J=11.7Hz, H-19b), 3.47(2H, t, J=6.4Hz, H-CO(CH 2 ) 2 C H 2 ),3.30(1H,dd,J=10.9,5.0Hz,H-3),2.55-2.41(3H,m,H-COC H 2 (CH 2 ) 2 ,11a),2.25-1.93(5H,m,H-1a,11a,-COCH 2 C H 2 CH 2 ),1.82-1.49(7H,m,H-1b,2,6,7a,9),1.20-0.95(11H,m,H-5,7b,17,18,20); IR(KBr,cm -1 )ν: 3553,3468,3103,2972,2945,2922,2868,1740,1715,1653,1445,1213,1132,1088,932,840,690,...
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