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Refinement method of arotinolol hydrochloride

A technology of alololol hydrochloride and refining method, which is applied in the field of chemical medicine, can solve the problems of lack of solutions, no cost advantage, cumbersome operation, etc., and achieve the effect of simple operation, control of solvent residue, and mild refining process

Active Publication Date: 2016-09-21
SHANDONG QIDU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, due to the poor solubility of arololol hydrochloride itself, researchers lack a suitable solution for its purification
The currently reported preparation methods are cumbersome to operate, the refining step uses a high boiling point solvent, the yield is low, and there is no cost advantage

Method used

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  • Refinement method of arotinolol hydrochloride
  • Refinement method of arotinolol hydrochloride
  • Refinement method of arotinolol hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 3 L reaction flask, add 1,100 ml of ethyl acetate, 220 ml of methanol, and 550 ml of purified water, add 55.0 g of arololol hydrochloride crude product under stirring, add weak base sodium carbonate powder to adjust the pH value to 10, and heat up to At about 32°C, stir until dissolved. Let stand to separate the liquids, and extract the aqueous phase with 275 ml of ethyl acetate once more. The organic phases were combined and washed with 500 ml of saturated sodium chloride solution. Add 20.0 g of sodium sulfate and dry for 0.5 h, filter, and concentrate to obtain an oil. Acetonitrile was added thereto, beating for 0.5 h, suction filtered, and dried to obtain 45.7 g of off-white solid, which was Arololol, with a yield of 91%.

[0031] Add 240 ml of methanol and 40.0 g of arololol to a 500 ml reaction flask, heat up and dissolve, add 0.8 g of activated carbon, continue to stir for 0.5 h, and filter with suction. Under stirring, add 20ml of 6 M hydrochloric acid so...

Embodiment 2

[0033] In a 3 L reaction flask, add 1,500 ml of ethyl acetate, 300 ml of methanol, and 750 ml of purified water, add 50.0 g of arololol hydrochloride crude product under stirring, add weak base sodium carbonate powder to adjust the pH value to 11, and heat up to At about 28°C, stir until dissolved. Let stand to separate the liquids, and extract the aqueous phase with 250 ml of ethyl acetate once more. The organic phases were combined and washed with 500 ml of saturated sodium chloride solution. Add 20.0 g of sodium sulfate and dry for 0.5 h, filter, and concentrate to obtain an oil. Methanol was added therein, beating for 0.5 h, suction filtered, and dried to obtain 40.1 g of off-white solid, namely Arololol, with a yield of 88%.

[0034] Add 320 ml of ethanol and 40.0 g of arololol to a 500 ml reaction flask. After heating up and dissolving, add 0.8 g of activated carbon, continue to stir for 0.5 h, and filter with suction. Under stirring, add 20 ml of 6 M hydrochloric aci...

Embodiment 3

[0036] In a 3 L reaction flask, add 1,350 ml of ethyl acetate, 210 ml of methanol, and 780 ml of purified water, add 52.0 g of arololol hydrochloride crude product under stirring, add weak base potassium carbonate powder to adjust the pH value to 11, and heat up to At about 30°C, stir until dissolved. Let stand to separate the liquids, and extract the aqueous phase with 260 ml of ethyl acetate once more. The organic phases were combined and washed with 500 ml of saturated sodium chloride solution. Add 20.0 g of sodium sulfate and dry for 0.5 h, filter, and concentrate to obtain an oil. Add ethanol to it, beat for 0.5 h, filter with suction, and dry to obtain 42.5 g of off-white solid, which is Arololol, with a yield of 90%.

[0037] Add 304 ml of methanol and 38.0 g of alololol to a 500 ml reaction flask, heat up and dissolve, add 1.0 g of activated carbon, continue to stir for 0.5 h, and filter with suction. Under stirring, 19 ml of 6 M hydrochloric acid solution was added...

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Abstract

The invention relates to a refinement method of arotinolol hydrochloride and belongs to the field of chemical medicines. The refinement method is characterized in that crude arotinolol hydrochloride is added to a system containing ethyl acetate, methanol and pure water, subjected to an alkali recovery operation under a weak alkaline condition, then pulped and purified, and free alkaline arotinolol with higher purity is obtained; arotinolol forms salt in an alcoholic solution, and refined arotinolol hydrochloride is obtained. The method is simple to operate, the yield is relatively high, and industrial production is facilitated.

Description

technical field [0001] The present invention belongs to the field of chemical medicine and relates to selectivity beta 1 - A process for refining the adrenoceptor antagonist arolol hydrochloride. . Background technique [0002] Arotinolol hydrochloride, a selective beta 1 - Adrenergic receptor antagonists, which were first launched in Japan in 1985, are mainly used clinically to treat mild to moderate essential hypertension, angina pectoris, tachyarrhythmia and essential tremor. In selective inhibition of β 1 - adrenergic receptors simultaneously, on alpha 1 -Adrenal receptors have a slight blocking effect, thereby reducing the tension of the sympathetic nerves, making the antihypertensive effect more ideal. [0003] In the disclosed technology at present, there are many literatures about the purification of arolol hydrochloride. The preparation method of arololol hydrochloride provided in the patent "a new method for the preparation of arololol hydrochloride (CN104530...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/04
CPCC07D417/04
Inventor 王孟孟凡领刘文坤张涛
Owner SHANDONG QIDU PHARMA
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