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Method for refining bevantolol hydrochloride

A technology of bevanolol hydrochloride and refining method, which is applied in the field of refining bevanolol hydrochloride, can solve the problems of increasing product cost, increasing solvent post-treatment work, difficult removal of inorganic salts, etc., to simplify operation and reduce refining times , the effect of controlling the content of inorganic salts

Inactive Publication Date: 2006-12-27
BEIJING SIHUAN KEBAO PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, we found in our experimental work that acetonitrile or isopropanol has no obvious refining effect on the color of this product and 3,4-dimethoxyphenethylamine hydrochloride, and it is difficult to remove inorganic salts
Using the refining method provided in the literature requires multiple recrystallizations of the product, which greatly increases the cost of the product and increases the post-processing work of the solvent

Method used

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  • Method for refining bevantolol hydrochloride
  • Method for refining bevantolol hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 150ml of distilled water and 50g of crude bevanolol hydrochloride to the reaction flask, reflux to dissolve the solid, heat filter, and cool the filtrate to crystallize. Suction filtration, drying to constant weight, white solid powder: 46g, yield: 92%, purity: 99.82% (HPLC), residue on ignition: 0.012%.

Embodiment 2

[0019] Add 2250ml of 5% isopropanol aqueous solution and 300g of crude product of bevanolol hydrochloride to the reaction flask, reflux to dissolve the solid, heat filter, and the filtrate is cooled and crystallized. Suction filtration, drying to constant weight, white solid powder: 282g, yield: 94%, purity: 99.81% (HPLC), residue on ignition: 0.010%.

Embodiment 3

[0021] Add 550 ml of 95% isopropanol aqueous solution and 100 g of crude bevanolol hydrochloride to the reaction flask, reflux to dissolve the solid, heat filter, and the filtrate is cooled and crystallized. Suction filtration and drying to constant weight gave white solid powder: 95g, yield: 95%, purity: 99.80% (HPLC), residue on ignition: 0.013%.

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Abstract

The invention relates to a high effective and low-cost method for refining bevantolol hydrochloride, the chemical construction of which is (1). It is a long-acting retardant for beta 1-acceptor, and is used for reducing blood pressure and treating angina pectoris.

Description

Technical field [0001] The invention relates to a method for refining bevanolol hydrochloride, which is a long-acting β 1 - Beta blockers, used to lower blood pressure and treat angina. Background technique [0002] Bevanolol hydrochloride (chemical name: 1-[2-(3,4-dimethoxyphenyl)ethylamino])-3-(3-methylphenoxy)-2-isopropanol hydrochloride ), has the following structure: [0003] [0004] Bevanolol hydrochloride is a long-acting beta 1 - Beta blockers, used to lower blood pressure and treat angina. [0005] According to existing literature, bevanolol hydrochloride is mainly synthesized according to the following route: [0006] [0007] The raw material 3,4-dimethoxyphenethylamine is used in the process, which forms a hydrochloride structure during the reaction process, which is difficult to separate from the final product by existing methods. The refining method of bevanolol hydrochloride mentioned in the literature mainly uses acetonitrile and isopropanol to re...

Claims

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Application Information

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IPC IPC(8): C07C217/60C07C213/10
Inventor 张志强谌伦华刘军华
Owner BEIJING SIHUAN KEBAO PHARM CO LTD
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