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
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Example Embodiment
[0020] Example 2
[0021] Add 3 g of irbesartan to the crystallizer, add 3 mL of tetrahydrofuran, and disperse the irbesartan in the solvent in a slurry state. Add 1.78 g of 40% hydrobromic acid and stir to complete the reaction. The ethyl acetate was added dropwise, and the amount of ethyl acetate added was 30 mL. Filter by suction and wash with ethyl acetate. The product was left to dry naturally at room temperature for 3 hours to obtain irbesartan hydrobromide, in which the mass percentage of water is 5%, and the characteristic X-ray powder diffraction peak positions of the product are expressed in 2θ as: 8.06, 10.94, 12.63 , 14.74, 15.06, 22.05, 22.86, 23.16, 26.47, 31.47. The DSC differential scanning calorimetry spectrum has two endothermic peaks, and the corresponding peak top temperatures are 139.5°C and 199.8°C, respectively.
Example Embodiment
[0022] Example 3
[0023] Add 3 g of irbesartan to the crystallizer, add 26 mL of acetone to dissolve the irbesartan. Add 1.97 g of 40% hydrobromic acid, stir to complete the reaction and the solution is clear. Start the dripping of cyclohexane until the crystals appear and stop the dripping. The crystals are grown for 15-20 minutes, and then the cyclohexane is added continuously. The amount of cyclohexane added is 250 mL in total. Filter by suction and wash with water. The product was dried at 90°C for 5 hours to obtain irbesartan hydrobromide, in which the mass percentage of water was 3.5%, and the powder diffraction results of the product were as follows figure 2 Shown. The DSC differential scanning calorimetry spectrum has two endothermic peaks, and the corresponding peak top temperatures are 138.0℃ and 198.3℃ respectively.
Example Embodiment
[0024] Example 4
[0025] Add 5 g of irbesartan to the crystallizer, add 20 mL of dioxane, and dissolve the irbesartan in the solvent. Add 2.36 g of 40% hydrobromic acid and stir to complete the reaction. Start adding 50 mL of ether dropwise. Filter by suction and wash with water. The product was dried at 50°C for 5 hours to obtain irbesartan hydrobromide, in which the mass percentage of water was 5%. The characteristic peak position of the product obtained by X-ray powder diffraction was expressed as 2θ: at 8.15, 11.07, 12.63, 14.61, 15.13, 22.16, 22.88, 23.26, 26.48, 31.55, and also include characteristic peaks at diffraction angles 2θ°=7.35, 13.99, 17.58, 17.97, 21.5, 28.1, 29.53. The DSC differential scanning calorimetry spectrum has two endothermic peaks, and the corresponding peak top temperatures are 140.0℃ and 198.3℃, respectively.
PUM
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap