Method for enriching, recovering and resolving alkaline chiral drug amlodipine from waste liquid

A chiral drug and basic technology, applied in the field of basic chiral drugs, to achieve the effect of high chiral separation efficiency, simple process, and high utilization rate of extractant

Pending Publication Date: 2020-05-05
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem of high-efficiency recovery of amlodipine and other basic chiral drugs in waste liquid, the present invention provides a kind of enrichment, recovery and resolution ammonium chloride with the advantages of high enrichment efficiency, large yield and high added value of products. The method of flat horizon

Method used

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  • Method for enriching, recovering and resolving alkaline chiral drug amlodipine from waste liquid
  • Method for enriching, recovering and resolving alkaline chiral drug amlodipine from waste liquid
  • Method for enriching, recovering and resolving alkaline chiral drug amlodipine from waste liquid

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Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: liquid-liquid extraction, aqueous phase crystallization and organic phase crystallization (see figure 1 ).

[0030] The method is divided into three steps: extraction and back-extraction enrichment of basic chiral drugs in the waste liquid (liquid-liquid extraction), aqueous phase crystallization recovery of basic chiral drugs in the back-extraction phase (aqueous phase crystallization), and alkali Organic phase crystallization chiral resolution of chiral drugs (organic phase crystallization). Taking amlodipine as a typical representative of basic chiral drugs is described in detail as follows: The first step—extraction and back-extraction enrichment of amlodipine in waste liquid: (1) Configure simulated waste liquid: weigh a certain amount of ammonia Dissolve lodipine or its racemate in water, adjust the pH to 6.0 with hydrochloric acid and sodium hydroxide, and prepare 200 mL of simulated waste liquid with an amlodipine concentration of 0.012 mol / L. (2...

Embodiment 2

[0031] Embodiment 2: liquid film extraction, aqueous phase crystallization and organic phase crystallization (see figure 2 , see the schematic diagram of the specific process Figure 4 ).

[0032] The method is divided into three steps: extraction and back-extraction enrichment of basic chiral drugs in the waste liquid (liquid membrane extraction), aqueous phase crystallization recovery of basic chiral drugs in the back-extraction phase (aqueous crystallization) and alkali Organic phase crystallization chiral resolution of chiral drugs (organic phase crystallization). Such as Figure 4 As shown, using amlodipine as a typical representative of basic chiral drugs is described in detail as follows: The first step—extraction and back-extraction enrichment of amlodipine in waste liquid: (1) Configure simulated waste liquid: weigh a certain A certain amount of amlodipine or its racemate was dissolved in water, and adjusted to pH=6.0 with hydrochloric acid and sodium hydroxide to...

Embodiment 3

[0033] Embodiment 3: aqueous phase crystallization and organic phase crystallization (see image 3 ).

[0034] The method is divided into two steps: crystallization recovery of basic chiral drugs in aqueous solution (aqueous phase crystallization) and organic phase crystallization chiral resolution of basic chiral drugs (organic phase crystallization). Taking amlodipine as a typical representative of basic chiral drugs is described in detail as follows: The first step - the crystallization recovery of amlodipine in aqueous solution: configure a simulated aqueous solution: weigh a certain amount of amlodipine or its racemate solution Dissolve in water with hydrochloric acid to prepare 20 mL of a simulated aqueous solution with a concentration of 0.12 mol / L of amlodipine. According to the molar ratio of amlodipine to L-tartaric acid=1:0.6, weigh L-tartaric acid and add a small amount of water to dissolve it, and add it to the aqueous solution containing amlodipine. Add sodium ...

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Abstract

The invention discloses a separation method for enriching, recovering and resolving an alkaline chiral drug (such as amlodipine) from a waste liquid. The method comprises the following three steps: extraction and back extraction enrichment (extraction) of the alkaline chiral drug in the waste liquid, water-phase crystallization recovery (water-phase crystallization) of the alkaline chiral drug ina back extraction phase, and organic-phase crystallization chiral resolution (organic-phase crystallization) of the alkaline chiral drug. Firstly, liquid-liquid extraction or liquid membrane extraction is adopted, and alkaline chiral drugs in waste liquid are extracted through an organic phase containing an acid extraction agent and then reversely extracted and enriched through a reverse extraction phase containing an acid reverse extraction agent. Then, an L-acid resolving agent is added into the reverse extraction phase, alkali is added to adjust the pH, and an alkaline chiral drug-L-acid resolving agent water-phase crystal substance is obtained; and finally, the water-phase crystal substance is dissolved in an organic solvent, a racemic alkaline chiral drug is added, organic-phase crystallization resolution is performed, and finally, resolution is performed to obtain optically pure R-alkaline chiral drug and S-alkaline chiral drug products.

Description

technical field [0001] The invention relates to a method for enriching, recovering and splitting amlodipine and other basic chiral drugs from waste liquid, and belongs to the technical field of chemical separation engineering. Background technique [0002] The human body is a highly asymmetric chiral environment. One enantiomer of many chiral drugs has curative effect on the human body, while the other enantiomer has no curative effect, and even has certain toxic and side effects. Amlodipine is a basic chiral drug, its full name is 6-methyl-2-(2-aminoethoxy)methyl-4-(2-chlorophenyl)-1,4-dihydro-3 , 5-methylethylpyridinedicarboxylate, is a dihydropyridine calcium channel antagonist, its racemate or left-handed enantiomer (S-amlodipine enantiomer) is widely used in the treatment of hypertension , coronary heart disease, angina pectoris and other cardiovascular and cerebrovascular diseases. Because of its definite curative effect, long half-life, stable and moderate antihyper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/90
CPCC07D211/90C07B2200/07C07B2200/13
Inventor 曾乐林刘潜易琴周媛唐课文
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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