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Preparation method of non-shaped obeticholic acid

An obeticholic acid and amorphous technology, applied in the field of preparation of amorphous obeticholic acid, can solve the problems of increased consumption of raw materials, high production cost, poor stability, etc., and achieve long-term preservation, good product stability, The effect of short production cycles

Active Publication Date: 2015-11-25
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the above-mentioned method for preparing amorphous obeticholic acid needs to use acid, alkali, etc., which not only increases the consumption of raw materials, but also produces a large amount of by-products such as sodium chloride, which brings difficulties to the separation and purification of the product. At the same time, the above-mentioned The method also has many defects such as many processes, cumbersome operation, high water content in the prepared product, poor stability, high production cost, etc., and is difficult to be applied in industry

Method used

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  • Preparation method of non-shaped obeticholic acid
  • Preparation method of non-shaped obeticholic acid
  • Preparation method of non-shaped obeticholic acid

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Experimental program
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Effect test

Embodiment 1

[0031] Obeticholic acid crystal form C samples were prepared according to US Patent US2013 / 0345188A1.

[0032] Dissolve 50.0g of crystal form C of obeticholic acid in 250ml of anhydrous methanol, and obtain a clear obeticholic acid solution after filtration; concentrate under reduced pressure to remove the solvent (vacuum degree is -0.08MPa; concentration temperature is 35°C) to obtain white obeticholic acid Cholic acid solid 49.0g, the yield is 98.0%; The solid is detected by X-powder diffraction as figure 1 shown.

Embodiment 2

[0034] Dissolve 50.0g of obeticholic acid crystal form C in 500ml of acetone, filter to obtain a clear obeticholic acid solution; concentrate under reduced pressure to remove the solvent (vacuum degree is -0.08MPa; concentration temperature is 35°C) to obtain white obeticholic acid Solid 49.2g, the yield is 98.4%; The solid is detected by X-powder diffraction as figure 1 shown.

Embodiment 3

[0036] Dissolve 50.0g of crystal form C of obeticholic acid in 500ml of ethyl acetate, and obtain a clear obeticholic acid solution after filtration; concentrate under reduced pressure to remove the solvent (vacuum degree is -0.08MPa; concentration temperature is 40°C) to obtain white obeticholic acid Cholic acid solid 49.3g, the yield is 98.6%; The solid is detected by X-powder diffraction as figure 1 shown.

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Abstract

The invention discloses a preparation method of non-shaped obeticholic acid. The preparation method comprises the following steps of a. dissolving the obeticholic acid into an organic solvent, and filtering, so as to obtain a filtering liquid, wherein the mass and volume ratio of the obeticholic acid and the organic solvent is 1:5-50g / ml; b. removing the solvent in the filtering liquid, so as to obtain the non-shaped obeticholic acid. The preparation method has the advantages that the water content of the prepared non-shaped obeticholic acid is low, the product stability is good, and the obeticholic acid product can be stored for a long time; the number of procedures is fewer, the operation is simple and convenient, the safety and environment-friendly effects are realized, the byproduct is avoided, the used solvent can be recycled and reutilized, the production cost is low, the production cycle is short, and the preparation method is very suitable for being applied into industry.

Description

technical field [0001] The invention relates to a preparation method of amorphous obeticholic acid. Background technique [0002] Obeticholic acid, also known as 6-ethylchenodeoxycholic acid, has a chemical name of 6α-ethyl-3α,7α-dihydroxy-5β-cholanic acid, and its molecular formula is C 26 h 44 o 4 , has the structure shown in formula 1, and can be used for treating primary biliary cirrhosis and nonalcoholic fatty liver disease. [0003] [0004] At present, obeticholic acid obtained by direct synthesis is usually crystalline obeticholic acid, such as: obeticholic acid crystal form C, F crystal form and G crystal form, etc. Due to the poor solubility of these crystal forms, it affects the drug’s efficacy. bioavailability and curative effect, so it is necessary to prepare these crystal forms into amorphous obeticholic acid to improve the solubility of obeticholic acid; for example, the method disclosed in US Patent US2013 / 0345188A1 and Chinese Patent CN104781272A is to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07B2200/13C07J9/005
Inventor 李大雄柯鸿樊小波孙毅
Owner CHENGDU BAIYU PHARMA CO LTD
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