Armiharisin succinic mono ester with cholagogic effect, and its salt and medicinal composition
A technology of succinic acid monoester and leucectin A, applied in the field of medicine, can solve the problems of reducing drug safety, toxic and side effects, etc.
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Embodiment 1
[0017] The preparation (method 1) of embodiment 1 leucidin A succinic acid monoester
[0018] Add 20g (0.085mol) of leucidin A, 46.9g (0.34mol) of anhydrous potassium carbonate, 300ml of ethyl acetate and 100ml of anhydrous N, N-dimethylformamide into a 500ml round-bottomed flask, oil bath 109 °C for 1 hour at reflux. A yellow solid gradually precipitated out of the reaction solution. Add 34 g (0.34 mol) of succinic anhydride, the solids in the reaction solution are partially dissolved, reflux for 30 hours, cool to room temperature, filter with suction, wash the obtained solid with a small amount of ethyl acetate, dissolve the filter cake in an appropriate amount of water, and wash with 10% hydrochloric acid Adjust to pH 3.5, stir for 0.5 hour, and filter with suction to obtain some products. Concentrate the filtrate to recover ethyl acetate, add 200 ml of water to the concentrate, adjust the pH to 3.5 with 10% hydrochloric acid, stir for 0.5 hour, and filter with suction to...
Embodiment 2
[0084] The preparation of embodiment 2 leucidin A succinate monoester sodium
[0085] Dissolve 1.67g (5mmol) succinic acid monoester of leucidin A in 60ml of methanol, add 0.42g (5mmol) sodium bicarbonate powder at room temperature under stirring, and stir at room temperature for 20 minutes to precipitate a large amount of yellow-green solid, continue to stir for reaction 3 After 1 hour, filter with suction, wash the filter cake with a small amount of methanol, and dry in vacuo to obtain 1.44 g of a yellow-green powdery solid, mp 197-198.5° C., yield 81%.
Embodiment 3
[0086] The preparation of embodiment 3 Leucidin A succinic acid monoester lysine salt
[0087] Dissolve 1.67g (5mmol) succinic acid monoester of leucectin A in 30ml tetrahydrofuran, add 0.82g (5mmol) lysine at room temperature under stirring, stir and react at room temperature for 12 hours, quickly filter to obtain a light yellow solid, immediately Transfer to a vacuum dryer, and vacuum-dry at 50°C for 4 hours to obtain 2.2g of the product, mp175-177°C, yield 90%.
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