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Preparation method of pharmaceutical armillarisin A

A kind of Leupillin A, pharmaceutical grade technology

Pending Publication Date: 2022-07-29
SHANXI YUNPENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because leucectin A is insoluble in water and very slightly soluble in ethanol, the yield is not high

Method used

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  • Preparation method of pharmaceutical armillarisin A

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preparation example Construction

[0032] A preparation method of pharmaceutical grade Leupillin A, the specific steps are as follows:

[0033] S1. take 3,5-dihydroxybenzyl alcohol and put it into the reaction flask, add ethanol and stir to dissolve, then add ethyl ethoxymethylene acetoacetate and stir to obtain solution A;

[0034] S2. Weigh sodium metal and dissolve it in ethanol to obtain sodium ethoxide;

[0035] S3. in the solution A obtained in S1, add the sodium ethoxide obtained in S2 to react, leave standstill, and filter to obtain solid A;

[0036] S4. react in S3 to obtain solid A and purified water to dissolve and add activated carbon for decolorization, and filter the activated carbon to obtain filtrate A;

[0037] S5. in the filtrate A that S4 obtains, add dropwise acid to adjust pH, filter to obtain leucovorin A crude product;

[0038] S6. the leucocidin A crude product obtained in S5 is placed in dehydrated alcohol and purified water mixed solution, after adding ammoniacal liquor to dissolve t...

Embodiment 1

[0052] Weigh 100g of 3,5-dihydroxybenzyl alcohol into a 2000mL reaction flask, add 1000g of absolute ethanol and stir until dissolved, add 150g of ethyl ethoxymethylene acetoacetate and stir to reach solution A for 40 minutes.

[0053] Weigh 21 g of metallic sodium and dissolve it in 450 g of anhydrous ethanol to obtain sodium ethoxide, add it to solution A, stir and react for 4 hours, stand for 12 hours and filter to obtain solid A.

[0054] The solid A was dissolved with 3000 g of purified water, 20 g of activated carbon was added for decolorization for 30 minutes, and the activated carbon was filtered to obtain filtrate A.

[0055] Filtrate A was added dropwise with dilute hydrochloric acid (60 g of hydrochloric acid and 60 g of purified water) to adjust the pH to 2. The temperature was lowered to 5°C for crystallization for 1 hour, and the crude leucovorin A was obtained by filtration.

[0056] 1500 g of absolute ethanol and 750 g of purified water were added to the leuco...

Embodiment 2

[0061]Weigh 100g of 3,5-dihydroxybenzyl alcohol into a 2000mL reaction flask, add 1000g of absolute ethanol and stir until dissolved, add 180g of ethyl ethoxymethylene acetoacetate and stir to reach solution A for 40 minutes.

[0062] Weigh 30 g of metallic sodium and dissolve it in 470 g of anhydrous ethanol to obtain sodium ethoxide, add it to solution A, stir and react for 4 hours, stand for 12 hours and filter to obtain solid A.

[0063] The solid A was dissolved with 3000 g of purified water, 20 g of activated carbon was added for decolorization for 30 minutes, and the activated carbon was filtered to obtain filtrate A.

[0064] Filtrate A was added dropwise with dilute hydrochloric acid (60 g of hydrochloric acid and 60 g of purified water) to adjust the pH to 2. The temperature was lowered to 5°C for crystallization for 1 hour, and the crude leucovorin A was obtained by filtration.

[0065] 1500 g of absolute ethanol and 750 g of purified water were added to the leucoc...

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Abstract

The invention relates to the technical field of pharmaceutical chemical preparation, in particular to a preparation method of pharmaceutical armillarisin A. The preparation method comprises the following specific steps: adding 3, 5-dihydroxybenzyl alcohol into ethanol, stirring and dissolving, adding ethoxymethylene ethyl acetoacetate, and stirring; dissolving metal sodium in ethanol to prepare sodium ethoxide; adding sodium ethoxide into the solution for reaction, standing and filtering to obtain a solid; dissolving the solid in purified water, adding activated carbon for decoloration, filtering to obtain filtrate, dropwise adding acid to adjust the pH value, and filtering to obtain an armillarisin A crude product; and putting the crude product into a mixed solution of absolute ethyl alcohol and purified water, adding ammonia water to dissolve the crude product, adding activated carbon to decolorize, filtering to obtain a filtrate, adding glacial acetic acid, cooling, crystallizing, filtering to obtain a refined armillarisin A product, and drying the refined product to obtain a finished armillarisin A product. Compared with the prior art, the method is simple in process operation, low in toxicity and high in yield, and the production cost can be further reduced. No catalyst is used, high-temperature and high-pressure reaction is avoided, reaction conditions are mild, and required equipment is simple.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical and chemical preparation, and more particularly, to a preparation method of pharmaceutical grade Leupillin A. Background technique [0002] Leupillin A, molecular formula: C 12 H 10 O 5 , Molecular weight: 234.2, Leucococcus A is a yellow or light yellow rectangular crystalline powder. Insoluble in water, very slightly soluble in ethanol and methanol; [0003] Structural formula: [0004] [0005] Leupillin A, also known as Pseudo Armillaria A, is a new coumarin compound, an active ingredient extracted from Pseudo Armillaria. It can promote bile secretion, relax the bile duct sphincter, reduce the tension of gastrointestinal smooth muscle, regulate the pressure of the bile duct system, promote the excretion of bile duct contents, regulate and promote immune function, and enhance the function of phagocytes. And can improve protein metabolism, regulate liver function. It is suitable...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/16
CPCC07D311/16
Inventor 孔攀锋
Owner SHANXI YUNPENG PHARMA
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