Preparation method of oleanolic acid derivatives
A technology for oleanolic acid and carboxylic acid compounds, which is applied in the field of preparation of oleanolic acid derivatives, can solve the problems of increasing production costs of enterprises, causing environmental pollution, and many side reactions, and achieves pollution avoidance, high yield, The effect of less by-products
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Embodiment 1
[0038] Example 1 : Synthesis of Compound Ⅰ-1
[0039]
[0040] 7.4 g of propionic acid was added to a reaction flask equipped with stirring, a condenser, and a thermometer, and 100 mL of dichloromethane was added. Add 19.2 g of EDC·HCl, then 16 g of triethylamine, stir at room temperature for a while, add 1.5 g of DMAP, stir for a while, then add 45.7 g of oleanolic acid, stir for reaction at room temperature, and control the reaction process by TLC. After the reaction, add appropriate amount of EDC·HCl 15.4g and triethylamine 12.8g, stir at room temperature for a period of time, then add 14.4g of 2-amino-4-carboxythiazole, continue the reaction at room temperature, and control the reaction process by TLC. After the reaction was completed, wash the reaction solution with 3×100 mL of dilute hydrochloric acid aqueous solution, then wash the reaction solution with 3×100 mL of saturated brine, dry, evaporate to dryness of dichloromethane, and refine with ethyl acetate-petroleu...
Embodiment 2
[0041] Example 2: Synthesis of Compound Ⅰ-2
[0042]
[0043] Add 8.8 g of butyric acid to a reaction flask equipped with stirring, a condenser, and a thermometer, and then add 100 mL of chloroform. Add 19.2 g of EDC·HCl, then 16 g of triethylamine, stir at room temperature for a while, add 1.5 g of DMAP, stir for a while, then add 45.7 g of oleanolic acid, stir for reaction at room temperature, and control the reaction process by TLC. After the reaction, add an appropriate amount of EDC·HCl 15.4g and triethylamine 12.8g, stir at room temperature for a period of time, then add 19.0g of 2-amino-4-phenyl-5-methylthiazole, and continue the reaction at room temperature. TLC controlled the progress of the reaction. After the reaction was completed, wash the reaction solution with 3×100 mL of dilute hydrochloric acid aqueous solution, then wash the reaction solution with 3×100 mL of saturated brine, dry, evaporate chloroform to dryness, and refine with ethyl acetate-petroleum ...
Embodiment 3
[0044] Example 3 : Synthesis of Compound Ⅰ-3
[0045]
[0046] 10.2 g of n-valeric acid was added to a reaction flask equipped with stirring, a condenser, and a thermometer, and then 100 mL of dichloromethane was added. Add 19.2 g of EDC·HCl, then 16 g of triethylamine, stir at room temperature for a while, add 1.5 g of DMAP, stir for a while, then add 45.7 g of oleanolic acid, stir for reaction at room temperature, and control the reaction process by TLC. After the reaction, add an appropriate amount of EDC·HCl15.4g and triethylamine 12.8g, stir at room temperature for a period of time, then add 16.8g of 2-amino-5-trifluoromethylthiazole, continue the reaction at room temperature, and control the reaction by TLC process. After the reaction was completed, wash the reaction liquid with 3×100 mL of dilute hydrochloric acid aqueous solution, then wash the reaction liquid with 3×100 mL of saturated brine, dry, evaporate to dryness of dichloromethane, and refine with ethyl ac...
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