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Refining method of tadalafil crystal form I

A technology of tadalafil and purification method, applied in chemical instruments and methods, other chemical processes, organic chemistry and other directions, can solve problems such as easy dispersion, difficulty in further improving the purity of tadalafil form I, and achieve increased binding site, increase the content of reducing groups, and reduce the effect of residues

Active Publication Date: 2022-07-05
NANJING ZENKOM PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] For the above-mentioned related technology, the inventor believes that although the solubility of tadalafil in water is improved by sodium lauryl sulfate in the related technology, it is easy to disperse in the organic phase and inorganic phase of sodium lauryl sulfate, It is also easy to combine with tadalafil molecules, making it difficult to further improve the purity of tadalamorph I

Method used

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  • Refining method of tadalafil crystal form I
  • Refining method of tadalafil crystal form I
  • Refining method of tadalafil crystal form I

Examples

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preparation example 1

[0038] In the present application, the adsorbent is prepared according to the following method: (1) Mix 4kg of zeolite powder with 8kg of silica sol with a water content of 86%, and leave it for 2 hours to obtain a modified liquid of zeolite powder;

[0039] (2) Mix the zeolite powder modified liquid with 0.8kg of silane coupling agent uniformly to obtain a mixed liquid, heat the mixed liquid in a water bath for 3 hours, then filter the mixed liquid, and dry the solid obtained by filtration to obtain an adsorbent; this step Among them, the silane coupling agent is γ-aminopropyltriethoxysilane.

[0040] As shown in Table 1, the difference between Examples 1-5 is that the weight of the raw materials used to prepare the adsorbent is different.

[0041]

preparation example 6-9

[0043] As shown in Table 2, the difference between Preparation Example 3 and Preparation Examples 6-9 is that the moisture content of the silica sol is different.

[0044]

preparation example 10

[0046] The difference between this preparation example and preparation example 7 is that the silane coupling agent is vinyltriethoxysilane.

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Abstract

The invention relates to the technical field of medicine refining, and particularly discloses a refining method of a tadalafil crystal form I. The preparation method comprises the following steps: (1) mixing a surfactant, acrylic acid, a tadalafil crude product and water, heating and stirring until the mixture is completely dissolved to obtain a tadalafil solution; (2) adding acetone and an antioxidant into the tadalafil solution, uniformly stirring, and adjusting the pH value of the solution to be neutral to obtain a preparation solution; and (3) adding an adsorbent and hydrogen peroxide into the preparation solution, stirring under the condition of ultraviolet irradiation, and then filtering, cooling and diluting, centrifuging, washing and drying to obtain the tadalafil crystal form I. According to the preparation method, dissolution of tadalafil in water is promoted through unsaturated fatty acid and acrylic acid, a mode of initiating free radical polymerization is adopted, the unsaturated fatty acid is removed while the adsorbent is removed, the residual quantity of the unsaturated fatty acid in the tadalafil amorphous form I is reduced, and the purity of the tadalafil amorphous form I is improved.

Description

technical field [0001] The present application relates to the technical field of pharmaceutical purification, and more specifically, to a purification method of Tadalamorph Form I. Background technique [0002] Tadalafil is a selective and reversible inhibitor of cyclic guanosine monophosphate (cGMP)-specific phosphodiesterase 5 (PDE5), which is widely used in medicine. At present, the preparation process of tadalafil mostly obtains crude tadalafil containing impurities, and the medicinal effect of crude tadalafil is relatively poor, so the crude tadalafil needs to be refined. [0003] There is a purification method of tadalafil crystal form I in the related art, which comprises the following steps: (1) adding sodium dodecyl sulfate and crude tadalafil into water, heating and stirring until completely dissolved; Add a solvent (the solvent is a mixture of isopropanol, acetonitrile and water) to the aqueous solution of crude dalafil and sodium dodecyl sulfate, heat and stir u...

Claims

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Application Information

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IPC IPC(8): C07D471/14B01J20/22B01J20/30
CPCC07D471/14B01J20/103B01J20/165B01J20/22C07B2200/13
Inventor 徐卓业陆荣政毛晓宇
Owner NANJING ZENKOM PHARMA
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