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Synthetic method of high-purity dopamine hydrochloride

A technology of dopamine hydrochloride and a synthesis method, applied in the field of medicinal chemistry, can solve the problems of many by-products, difficult to realize industrial production, difficult to purify, etc., and achieves the effects of less three wastes and simple post-processing method.

Active Publication Date: 2020-11-06
山东达冠医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of this route uses enzymes as catalysts, the reaction conditions are harsh, and the price of enzymes is high, the reaction yield is low, and the product purity is low, there are many by-products, purification is difficult, it is not conducive to cost control, and it is difficult to realize industrial production.

Method used

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  • Synthetic method of high-purity dopamine hydrochloride
  • Synthetic method of high-purity dopamine hydrochloride
  • Synthetic method of high-purity dopamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Mix 3.4-dimethoxyphenethylamine (200.0g, 1.10mol) with 800ml of ethanol, add dropwise 204.0g (1.21mol) of hydrobromic acid with a concentration of 48%, control the internal temperature not higher than 50°C, add dropwise After completion, the reaction was stirred for 0.5 hours. Stir and cool down to 20-30°C for crystallization for 2 hours, filter to obtain the crude product of 3,4-dimethoxyphenethylamine hydrobromide, recrystallize the wet product with absolute ethanol, filter, and air-dry to obtain a white powder Solid 3.4-dimethoxyphenethylamine hydrobromide 196.7g, purity 99.84%, yield 68.2%;

[0036] Mix 196.7 g of 3.4-dimethoxyphenethylamine hydrobromide with 1573.6 g of 48% hydrobromic acid, replace with nitrogen, and heat to an internal temperature of 110-115° C. for 5 hours. Turn off the heating, stir and cool down to 20-30°C for crystallization for 2 hours, filter, and vacuum-dry to obtain 146.0 g of white solid dopamine hydrobromide with a purity of 99.92% and...

example 2

[0039] Mix 3.4-dimethoxyphenethylamine (200.0 g, 1.10 mol) with 600 ml of isopropanol, add hydrochloric acid (223.0 g, 2.20 mol) dropwise in a water bath to control the internal temperature not higher than 50 °C, and dropwise is completed. Evaporate the solvent, add 600ml of ethyl acetate, stir and crystallize, filter to obtain a light yellow solid, add absolute ethanol to recrystallize, filter, and blow dry to obtain 170.5g of white powdery solid 3.4-dimethoxyphenethylamine hydrochloride , purity 99.81%, yield 71.2%;

[0040] Mix 170.5 g of 3.4-dimethoxyphenethylamine hydrochloride with 1023.0 g of 40% hydrobromic acid, replace with nitrogen, and heat to an internal temperature of 100-110° C. for 5 hours. Turn off the heating, stir and cool down to 20-30°C for crystallization for 2 hours, filter, and vacuum-dry to obtain 139.5 g of white solid dopamine hydrobromide with a purity of 99.83% and a yield of 76.1%;

[0041] Mix 139.5 g of dopamine hydrobromide with 1116 ml of abs...

example 3

[0043]Mix 3.4-dimethoxyphenethylamine (200.0g, 1.10mol) with 800ml of isopropanol, add dropwise 48% hydrobromic acid (222.5g, 1.32mol) to control the internal temperature not higher than 50°C, and dropwise , stirred and cooled to 20-30 ° C for 2 hours, filtered to obtain a light yellow solid, added absolute ethanol to recrystallize, filtered, and air-dried to obtain a white powdery solid 3.4-dimethoxyphenethylamine hydrobromide 192.3 g, purity 99.82%, yield 66.7%;

[0044] Mix 192.3 g of 3.4-dimethoxyphenethylamine hydrobromide with 961.5 g of 48% hydrobromic acid, replace with nitrogen, and heat to an internal temperature of 110-120° C. for 5 hours. Turn off the heating, stir and cool down to 20-30°C for crystallization for 2 hours, filter, and vacuum-dry to obtain 136.2 g of white solid dopamine hydrobromide with a purity of 99.85% and a yield of 79.3%;

[0045] Mix 136.2 g of dopamine hydrobromide with 1,089.6 ml of isopropanol, replace with nitrogen, heat up to 80° C. and...

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PUM

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Abstract

The invention provides a synthetic method of dopamine hydrochloride, and belongs to the field of drug synthesis. The preparation method comprises the following steps: taking 3,4-dimethoxyphenylethylamine as an initial raw material, firstly reacting with an acid to form a salt, re-crystallizing and refining to obtain 3,4-dimethoxyphenylethylamine salt, reacting with hydrobromic acid to remove methyl to generate dopamine hydrobromide, and finally reacting with hydrochloric acid to form a salt so as to obtain dopamine hydrochloride. The preparation method provided by the invention has the advantages of cheap and easily available initial raw materials, simple process, no high-temperature and high-pressure hydrogenation step, low cost, high purity and high yield, and is suitable for industrialproduction.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, in particular to a method for synthesizing high-purity dopamine hydrochloride. Background technique [0002] Dopamine Hydrochloride (Dopamine Hydrochloride), chemical name 4-(2-aminoethyl)-1,2-benzenediol hydrochloride. Dopamine has β-receptor stimulant effect, and also has certain α-receptor stimulant effect, which can enhance myocardial contractility, increase cardiac output, increase heart rate slightly, have mild contraction effect on peripheral blood vessels, increase arterial pressure, and Visceral blood vessels expand, increase blood flow, increase renal blood flow and glomerular filtration rate, thereby increasing urine output and sodium excretion, improving peripheral circulation, significantly increasing urine output, and having no significant effect on heart rate. Because of its superiority over other vasoconstrictors or vasodilators, it can be used clinically for various ...

Claims

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Application Information

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IPC IPC(8): C07C213/08C07C215/52C07C213/10
CPCC07C213/08C07C213/06C07C213/10C07C217/60C07C215/52
Inventor 盛遵田邓义蒙田成艳刘发文李广乾王海峰尹凤学丁凤娟杨荣
Owner 山东达冠医药科技有限公司
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