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Irbesartan hydrobromide and preparation method thereof

A hydrobromide, hydrobromic acid technology, applied in metabolic diseases, cardiovascular system diseases, urinary system diseases and other directions, can solve the problems such as product purity and particle size cannot be well controlled, and achieve the advantages of industrial operation, The effect of smooth surface and cost reduction

Inactive Publication Date: 2010-07-21
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since there is no recrystallization process after dissolution, the purity and particle size of the product cannot be well controlled

Method used

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  • Irbesartan hydrobromide and preparation method thereof
  • Irbesartan hydrobromide and preparation method thereof
  • Irbesartan hydrobromide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0021] 3g of irbesartan was added to the crystallizer, and 3mL of tetrahydrofuran was added to disperse the irbesartan in a slurry form in the solvent. Add 1.78 g of 40% hydrobromic acid and stir to complete the reaction. Begin to add ethyl acetate dropwise, and the amount of ethyl acetate added is 30 mL in total. Suction filtration, ethyl acetate washing. The product was left to dry naturally at room temperature for 3 hours to obtain irbesartan hydrobromide, wherein the mass percentage of water was 5%, and the X-ray powder diffraction characteristic peak positions of the product were expressed in 2θ as: 8.06, 10.94, 12.63 , 14.74, 15.06, 22.05, 22.86, 23.16, 26.47, 31.47. There are two endothermic peaks in DSC differential scanning calorimetry, and the corresponding peak top temperatures are 139.5°C and 199.8°C, respectively.

Embodiment 3

[0023] 3g of irbesartan was added to the crystallizer, and 26mL of acetone was added to dissolve the irbesartan. Add 1.97 g of 40% hydrobromic acid, stir to make the reaction complete, and the solution is clear. Start to add cyclohexane dropwise until the crystals come out, stop the dropwise addition, grow the crystals for 15-20 minutes, then continue to add cyclohexane, the amount of cyclohexane added is 250mL in total. Suction filtration, washing with water. The product was dried at 90°C for 5 hours to obtain irbesartan hydrobromide, wherein the mass percentage of water was 3.5%, and the powder diffraction results of the product were as follows: figure 2 shown. There are two endothermic peaks in DSC differential scanning calorimetry, and the corresponding peak top temperatures are 138.0°C and 198.3°C, respectively.

Embodiment 4

[0025] 5g of irbesartan was added to the crystallizer, 20mL of dioxane was added, and irbesartan was dissolved in the solvent. Add 2.36 g of 40% hydrobromic acid and stir to complete the reaction. Start to add ether 50mL dropwise. Suction filtration, washing with water. The product was dried at 50°C for 5 hours to obtain irbesartan hydrobromide, wherein the mass percentage of water was 5%, and the position of the characteristic peak obtained by X-ray powder diffraction of the product was expressed in 2θ as: at 8.15, 11.07, 12.63, 14.61, 15.13, 22.16, 22.88, 23.26, 26.48, 31.55, and also contain characteristic peaks at diffraction angles 2θ°=7.35, 13.99, 17.58, 17.97, 21.5, 28.1, 29.53. There are two endothermic peaks in DSC differential scanning calorimetry, and the corresponding peak temperatures are 140.0°C and 198.3°C, respectively.

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Abstract

The invention relates to irbesartan hydrobromide and a preparation method thereof; irbesartan and solvent are mixed to prepare into solution or suspension liquid, and the mass ratio of the solvent volume and the irbesartan is 1-10mL / g; and then the solution or suspension liquid is mixed with hydrobromic acid solution, and the mass ratio of the hydrobromic acid in the hydrobromic acid solution andthe irbesartan is 1:2.6-5.3; the mixture is stirred continuously, after the solution is settled, elution agent is dropwise added, the volume ratio of the elution agent and the solvent is 1-10:1, seedcrystal is added or crystal growing is carried out after crystal generation is carried out spontaneously, after the elution agent is dropwise added, crystal mush is washed and dried to obtain the irbesartan hydrobromide after solid-liquid separation is carried out. The irbesartan hydrobromide obtained in the invention has adjustable granularity, concentrated granularity distribution, bright and clean surface, good product mobility, high crystallinity and low static electricity property, and is beneficial to industrial operation; in addition, the product has stable performance, is hard to be decomposed and is convenient for storage and transportation and usage.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical crystallization, and relates to irbesartan hydrobromide and a preparation method thereof. Background technique [0002] Irbesartan (irbesartan), the chemical name is 2-butyl-3-[4-[2-(1H-tetrazol-5-yl)phenyl]benzyl]-1,3-diazaspiro- [4.4] Non-1-en-4-one, white crystalline powder. Irbesartan belongs to non-peptide angiotensin II receptor (AT subtype) blocker, through the inhibition of angiotensin II receptor (AT1), it can completely block the blood vessels mediated by AT1 receptor The full activity of tensin I inhibits the vasoconstriction mediated by angiotensin II; inhibits the reabsorption of renal tubular sodium mediated by angiotensin II and promotes the release of aldosterone, and inhibits the response of RAS to pressure receptor reflex in the brain Regulating, increasing the sensitivity of this reflex; inhibiting the action of angiotensin II on stimulating intravascular sympathetic ne...

Claims

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Application Information

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IPC IPC(8): C07D403/10A61P9/12A61P9/04A61P13/12A61P3/10
Inventor 王静康鲍颖张美景尹秋响王林侯宝红龚俊波王永莉陈巍
Owner TIANJIN UNIV
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