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Dexrabeprazole sodium monohydrate crystal form and preparation method thereof

A technology of dex-rabeprazole sodium and rabeprazole sodium, which is applied in the field of dex-rabeprazole sodium monohydrate crystal form and its preparation, can solve the problems of strong hygroscopicity, dissolution rate, stability and solubility low hygroscopicity, simple preparation method and good stability

Inactive Publication Date: 2014-09-10
HAINAN HAILI PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] U.S. Patent US2009018249 reports on rabeprazole sodium, potassium, magnesium, lithium, calcium and zinc salts and the crystal form and amorphous properties of these salts, as well as the research on the crystal form and amorphous properties of rabeprazole, European invention patent EP1935891 reported the crystalline hydrated form γ of rabeprazole sodium and its preparation method by adding seed crystals in a polar aprotic solvent, and pointed out that the crystalline form γ is thermodynamically more stable than the known hydrated forms α and β. Chinese patent CN102924434A A crystal form of dex-rabeprazole sodium monohydrate and its preparation method are mentioned, and a new crystal form of rabeprazole sodium is recorded, which is determined by X-ray powder diffraction measurement method, using Cu-Kα radiation, The X-ray powder diffraction spectrum represented by 2θ angle has characteristic diffraction peaks at about 10.5°, 13.4°, 17.1°, 18.0°, 18.5°, 18.9°, 19.5°, 23.0°, 23.3°, 27.1°, 31.6°; DSC shows that the endothermic peak is 148.27°C; amorphous dex-rabeprazole sodium has strong hygroscopicity, and has disadvantages such as poor dissolution rate, stability and solubility. Therefore, obtaining a stable crystalline form of dex-rabeprazole sodium is very necessary

Method used

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  • Dexrabeprazole sodium monohydrate crystal form and preparation method thereof
  • Dexrabeprazole sodium monohydrate crystal form and preparation method thereof
  • Dexrabeprazole sodium monohydrate crystal form and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Synthesis of dex-rabeprazole sodium monohydrate crystals

[0039] Add 2.0 g of sodium hydroxide to 10 ml of acetonitrile, stir, add 15 g of dex-rabeprazole into the resulting solution and stir to dissolve, filter the resulting solution, concentrate to dryness, vacuumize for 8 hours, and add the resulting concentrate to 10 ml of methanol , stirred to dissolve, filtered, concentrated to dryness under reduced pressure, added the obtained concentrate to 10ml ethyl acetate, stirred and crystallized at room temperature for 12h, filtered under nitrogen protection, washed the filter cake with ethyl acetate, dried in vacuum at 40°C for 24h to obtain off-white Dexrabeprazole sodium monohydrate crystal form. The obtained solid X-ray powder diffraction pattern is as follows figure 1 , the differential scanning calorimetry diagram is shown in figure 2 , infrared spectrum such as image 3 , indicating that the obtained compound is a crystalline form. The water content of the com...

Embodiment 2

[0041] Synthesis of dex-rabeprazole sodium monohydrate crystals

[0042]Add 2.0 g of sodium hydroxide to 10 ml of acetonitrile, stir, add 15 g of dex-rabeprazole into the resulting solution and stir to dissolve, filter the resulting solution, concentrate to dryness, vacuumize for 8 hours, and add the resulting concentrate to 10 ml of acetonitrile , stir to dissolve, filter, concentrate to dryness under reduced pressure, add the obtained concentrate to 10ml ethyl acetate, stir and crystallize at room temperature for 12h, filter under nitrogen protection, wash the filter cake with ethyl acetate, and vacuum dry at 40°C for 24h to obtain off-white Dexrabeprazole sodium monohydrate crystal form. The resulting solid had the same physical properties as the product obtained in Example 1.

Embodiment 3

[0044] Synthesis of dex-rabeprazole sodium monohydrate crystals

[0045] Add 2.0g of sodium hydroxide to 10ml of acetonitrile, stir, add 15g of dex-rabeprazole into the obtained solution and stir to dissolve, filter the obtained solution, concentrate to dryness, vacuumize for 8h, and add the obtained concentrate into 10ml of acetone , stir to dissolve, filter, concentrate to dryness under reduced pressure, add the obtained concentrate to 10ml ethyl acetate, stir and crystallize at room temperature for 12h, filter under nitrogen protection, wash the filter cake with ethyl acetate, and vacuum dry at 40°C for 24h to obtain off-white Dexrabeprazole sodium monohydrate crystal form. The resulting solid had the same physical properties as the product obtained in Example 1.

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Abstract

The invention provides a dexrabeprazole sodium monohydrate crystal form. In an X-ray powder diffraction spectrum obtained through Cu-K<alpha> radiation and represented by 2<theta> angles, the dexrabeprazole sodium monohydrate crystal form has characteristic diffraction peaks at 9.2 DEG, 10.6 DEG, 17.1 DEG, 18.0 DEG, 18.5 DEG, 18.8 DEG, 19.5 DEG, 21.3 DEG, 21.5 DEG, 22.9 DEG, 25.4 DEG, 27.1 DEG, 29.8 DEG, 31.6 DEG and 32.6 DEG; in a differential thermal analysis spectrum, the dexrabeprazole sodium monohydrate crystal form has an absorption peak at 157.4 DEG. The crystal form has good stability, good solubility, a good dissolution rate and low moisture absorption. The invention also provides a preparation method for the dexrabeprazole sodium monohydrate crystal form, and the method has the advantages of high yield, simple operation, low cost and suitability for industrialized production.

Description

technical field [0001] The present invention relates to (R)-2-[[[4-(3-methoxypropoxy)-3-methylpyridin-2-yl]methyl]sulfinyl]-1H-benzimidazole sodium ( D-rabeprazole sodium) monohydrate crystal form and preparation method thereof. Background technique [0002] Sodium Rabeprazole (Sodium Rabeprazole) is a new type of proton pump inhibitor, which can be used in the treatment of acid-related diseases, such as peptic ulcer, gastroesophageal reflux disease, Zoller-Ellison syndrome, etc. Compared with other proton pump inhibitors currently on the market, rabeprazole sodium has a more significant ability to relieve symptoms, and its adverse reactions are milder. [0003] Rabeprazole sodium contains two optical isomers, left-handed and right-handed. Dextral Rabeprazole Sodium (DextralRabeprazole Sodium) is the right-handed isomer of rabeprazole sodium. The chemical name is (R)-2-[ [[4-(3-methoxypropoxy)-3-methylpyridin-2-yl]methyl]sulfinyl]-1H-sodium benzimidazole, its structural fo...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 宋力余国新
Owner HAINAN HAILI PHARMACEUTICAL CO LTD
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