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Method for preparing high-purity benidipine hydrochloride

A benidipine hydrochloride, high-purity technology, applied in the field of medicine, can solve problems such as time-consuming and labor-intensive consumption, large consumption of organic solvents, adverse effects of environmental protection, etc., and achieve the effect of simplifying steps, saving manpower and material resources, and easy operation

Inactive Publication Date: 2012-10-24
张兆勇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above-mentioned separation method is a multi-step operation, and even column chromatography is required to effectively separate the isomers. Adverse effects of

Method used

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  • Method for preparing high-purity benidipine hydrochloride
  • Method for preparing high-purity benidipine hydrochloride
  • Method for preparing high-purity benidipine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Under ultrasonic conditions, take the main ring of dihydropyridine [2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl ester] 10 grams into a 200mL reaction flask, add 14mL N,N-dimethylformamide (DMF) and 56mL dichloromethane, add 2.4mL thionyl chloride to the obtained homogeneous suspension under ice-bath cooling, and stir for 1 hour to obtain Clear solution.

[0020] Then 6.3 g of pyridine (alcohol) side chain [1-benzyl-3-hydroxypiperidine] was added, and the stirring reaction was continued for 2.5 hours under ice-cooling.

[0021] The reaction solution was washed four times with 40 mL of water and once with 40 mL of saturated brine, and dried with 4 g of anhydrous sodium sulfate in the dichloromethane liquid for 2 hours, filtered to remove the solid sodium sulfate, and recovered the dichloromethane under reduced pressure to obtain yellow to red coarse crystals , hereinafter referred to as benidipine hydrochloride coarse crystals.

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Embodiment 2

[0024] 3.0 g of 3-nitrobenzaldehyde, 2.6 g of ethyl β-aminocrotonate and 2.6 g of ethyl acetoacetate were dissolved in 10 mL of DMF and 50 mL of dichloromethane mixed solvent, and stirred at 50°C for 3 h. After washing with water, drying, and recovering the solvent, benidipine hydrochloride was obtained as yellow to red coarse crystals.

Embodiment 3

[0026] Take 10 grams of benidipine hydrochloride coarse crystals, dissolve them in 60 mL of acetone, ultrasonicate for 8 minutes under 200 W, 80 MHz ultrasonic conditions, filter with suction, then dissolve the above-mentioned crystals under reflux under 5 mL of ethanol, and add 40 mL of acetone, sonicated for 8 minutes, suction filtered, and dried to obtain 3.2 g of light yellow powder crystals.

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Abstract

The present invention relates to a production method of benidipine hydrochloride (+ / -)-(R*)-1,4-dihydro-2,6-dimethyl-4-(m-nitrophenyl)-3,5-picolinic acid methyl ester [(R*)-1-benzyl-3-piperidine alcohol ester] hydrochloride. Specifically, the method is as below: 1) benidipine hydrochloride is directly synthesized through dihydropyridine main ring chlorination and then linkage with a side chain; and an ultrasound technology is introduced in a pretreatment stage to disperse and dissolve reaction raw materials through ultrasonic, so as to increase speed of reaction; and 2) an ultrasound technology is introduced in a post-treatment stage, and the benidipine hydrochloride coarse grain (or dried reaction products) obtained from the above method or other possible synthesis routes is dissolved and prepared into high-purity benidipine hydrochloride by ultrasonic.

Description

technical field [0001] The invention relates to the technical field of medicine, and is a process for preparing high-purity benidipine hydrochloride by introducing ultrasonic technology, specifically: 1) after the main ring of dihydropyridine is acyl chlorinated, it is then linked with the side chain, directly In the pretreatment stage of synthesizing benidipine hydrochloride, ultrasonic technology is introduced to disperse and dissolve the reaction raw materials through ultrasonic dispersion, so as to increase the reaction speed. 2) In the post-treatment stage, ultrasonic technology is introduced to obtain high-purity crystals of benidipine hydrochloride (or the reaction product after evaporation) obtained by the above-mentioned method or other possible synthetic routes, and then obtained by ultrasonication after redissolving. crystallization of benidipine hydrochloride. Background technique [0002] The chemical name of benidipine hydrochloride is (±)-(R*)-1,4-dihydro-2,6...

Claims

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Application Information

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IPC IPC(8): C07D211/90
CPCC07D401/12A61P9/10A61P9/12
Inventor 张兆勇
Owner 张兆勇