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Dexlansoprazole crystal form and preparation method

A technology of dexlansoprazole crystals and crude dexlansoprazole, which is applied in the field of dexlansoprazole crystal forms and preparation, can solve problems such as product instability, and achieve long-term storage convenience and clinical drug safety , the effect of high drug safety

Inactive Publication Date: 2017-06-20
SHANDONG YUXIN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN102875531B discloses the crystalline form product obtained by heating and dissolving the raw material of dexlansoprazole in ethyl acetate, n-heptane, diethylamine system and then cooling down to crystallize, but the crystal form obtained by the applicant using this patent method Stability has the problem of product instability in industrial applications, so it is necessary to strive to find a stable crystal form of D-lansoprazole

Method used

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  • Dexlansoprazole crystal form and preparation method
  • Dexlansoprazole crystal form and preparation method
  • Dexlansoprazole crystal form and preparation method

Examples

Experimental program
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Embodiment 1

[0024] The preparation of embodiment 1 dexlansoprazole crystal form

[0025] In the 1000ml flask, add 10g dexlansoprazole crude product, 100ml acetone, stir and dissolve. Add 0.5 g of activated carbon, stir and decolorize for 0.5 hours, and filter. Control the temperature at 20° C., add 40 ml of isopropyl ether to the filtrate, stir and grow the crystals for 0.5 hours, tiny crystals appear, and the solution becomes turbid. Continue to dropwise add 300ml of isopropyl ether, and the dropwise addition is completed in 3 hours. It was filtered and vacuum-dried to obtain 8.99 g of white crystalline powder with an HPLC purity of 99.91%.

[0026] Prepared dexlansoprazole is measured by powder X-ray diffractometry method, obtains X-ray powder diffraction collection of patterns such as figure 1 shown.

[0027] Using the PE Pyris Diamond TG thermogravimetric analyzer of Perkin-Elmer Company in the United States, the thermogravimetric analysis spectrum is as follows figure 2 As show...

Embodiment 2

[0028] The preparation of embodiment 2 dexlansoprazole crystal forms

[0029] In the 1000ml flask, add 10g dexlansoprazole crude product, 100ml acetone, stir and dissolve. Add 0.5 g of activated carbon, stir and decolorize for 0.5 hours, and filter. Control the temperature at 20° C., add 60 ml of isopropyl ether to the filtrate, stir and grow the crystals for 1 hour, tiny crystals appear, and the solution becomes turbid. Continue to dropwise add 350ml of isopropyl ether, and the dropwise addition is completed in 3 hours. It was filtered and vacuum-dried to obtain 9.21 g of white crystalline powder with an HPLC purity of 99.97%.

[0030] According to the XPRD data, the obtained crystal form is consistent with the crystal form in Example 1. The thermogravimetric analysis spectrum obtained by using the PEPyris Diamond TG thermogravimetric analyzer of Perkin-Elmer Company of the United States is consistent with that of Example 1.

Embodiment 3

[0031] The preparation of embodiment 3 dexlansoprazole crystal forms

[0032] In the 1000ml flask, add 10g dexlansoprazole crude product, 100ml acetone, stir and dissolve. Add 0.5 g of activated carbon, stir and decolorize for 0.5 hours, and filter. Control the temperature at 20° C., add 70 ml of isopropyl ether to the filtrate, stir and grow the crystals for 0.5 hours, tiny crystals appear, and the solution becomes turbid. Continue to dropwise add 300ml of isopropyl ether, and the dropwise addition is completed in 3 hours. It was filtered and vacuum-dried to obtain 9.08 g of white crystalline powder with an HPLC purity of 99.93%.

[0033] According to the XPRD data, the obtained crystal form is consistent with the crystal form in Example 1. The thermogravimetric analysis spectrum obtained by using the PEPyris Diamond TG thermogravimetric analyzer of Perkin-Elmer Company of the United States is consistent with that of Example 1.

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Abstract

The invention belongs to the technical field of medicines and in particular relates to a dexlansoprazole crystal form and a preparation method. A dexlansoprazole crystal with good heat stability is obtained through a method comprising the steps of culturing a crystal nucleus and slowly crystallizing. The preparation method comprises the following steps: dissolving an anhydrous dexlansoprazole crude product into acetone and de-coloring with active carbon; dropwise adding one part of isopropyl ether at 20 DEG C to 25 DEG C; stirring and culturing a crystal; culturing the crystal nucleus; then slowly dropwise adding the other part of isopropyl ether; filtering and drying to obtain a product. The product prepared by the method provided by the invention is good in heat stability and slow in degradation speed; the problems of degradation, color change and the like during a storage process of the dexlansoprazole are effectively solved; the solubility and dissolvability of the product prepared by the method are also extremely improved and the bioavailability is improved.

Description

technical field [0001] The invention relates to a crystal form of dexlansoprazole and a preparation method thereof. Background technique [0002] Dexlansoprazole is a novel proton pump inhibitor, the dextroenantiomer of lansoprazole, developed by Takeda Pharmaceutical Company of Japan for the treatment of gastric cancer associated with non-erosive gastroesophageal reflux disease Burning and varying degrees of erosive esophagitis. The chemical structure is as follows: [0003] [0004] Proton pump inhibitors are benzimidazole derivatives that specifically and non-competitively act on H+ / K+-ATPase to treat peptic ulcer. Proton pump inhibitors are mostly fat-soluble and weakly alkaline. After being absorbed into the blood, they enter the acidic environment in the parietal cell secretory tubules and tubule vesicles. The activated products are generally active sulfenic acid and sulfenamide, which interact with H+-K+-ATPase Sulfhydryl coupling forms an irreversible covalent ...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07D401/12C07B2200/13
Inventor 孔磊夏军吕秀生
Owner SHANDONG YUXIN PHARMA CO LTD
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