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A kind of preparation method of desloratadine

A technology of desloratadine and loratadine, which is applied in the field of drug synthesis, can solve the problems of low product purity and unsuitability for clinical application, and achieve the effects of improving purity, reducing side reactions, and strong operability

Active Publication Date: 2017-02-01
GUANGDONG JIUMING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For this reason, the technical problem to be solved by the present invention is that the method for preparing desloratadine in the prior art has the problem of low product purity, which is not suitable for direct clinical application, and then provides a method for preparing desloratadine with high purity Methods

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  • A kind of preparation method of desloratadine
  • A kind of preparation method of desloratadine
  • A kind of preparation method of desloratadine

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preparation example Construction

[0028] The preparation routes of the following examples of the present invention are as follows:

[0029]

Embodiment 1

[0031] The preparation method of desloratadine described in the present embodiment comprises the following steps:

[0032](1) get loratadine 15kg (39.17mol) shown in formula A-I and be dissolved in the ethanol solvent that volume concentration is 75% in the ethanol solvent of 138L under nitrogen protection, then add potassium hydroxide 30kg (535.7mol) and stir evenly, and Rapidly raise the temperature to 70-75°C to start the reflux reaction, and then control the reflux reaction to show a gradient change within 70-100°C until the loratadine reaction is complete. The gradient temperature change program of the reflux reaction is specifically: Rapidly raise the reaction temperature from 75°C to 80°C, and keep the reaction for 3h; then quickly raise the temperature to 100°C, and keep the reaction for 2h; then quickly cool down to 85°C, and keep the reaction for 3h; then quickly cool down to 70°C, until the reaction completely;

[0033] Detect whether the loratadine reaction is com...

Embodiment 2

[0039] The preparation method of desloratadine described in the present embodiment comprises the following steps:

[0040] (1) 15kg (39.17mol) of loratadine shown in formula A-I is dissolved in the methanol solvent of 55% volume concentration in 163L of methanol solvent under the protection of nitrogen, then add potassium hydroxide 60kg (1071.4mol) and stir evenly, and Rapidly raise the temperature to 70-75°C to start the reflux reaction, and then control the reflux reaction to show a gradient change within 70-100°C until the loratadine reaction is complete. The gradient temperature change program of the reflux reaction is specifically: Rapidly raise the reaction temperature from 75°C to 100°C, and keep the reaction for 2h; then quickly cool down to 85°C, and keep the reaction for 2h; then quickly raise the temperature to 100°C, and keep the reaction for 3h; Complete response;

[0041] Detect whether the loratadine reaction is complete with thin-layer chromatography, specific...

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Abstract

The invention relates to a preparation method of desloratadine. The preparation method comprises the following steps: (1) dissolving loratadine into an alcohol solvent with the volume concentration of 55-75% under the protection of nitrogen, adding potassium hydroxide, heating to 70-75 DEG C, beginning reflux reaction, controlling the temperature of the reflux reaction to keep a gradient change within 70-100 DEG C, and refluxing till complete reaction of the loratadine; (2) adding an ethyl acetate solvent into a completely reacted reaction solution for extracting, draining out a water layer, repeating the extracting step for 2-3 times, washing by using water, and crystallizing, decolorizing and recrystallizing to obtain desloratadine. By the preparation method, the technical problems that in the prior art, the product desloratadine cannot meet a requirement for purity, contains many impurities, and cannot meet requirements on clinical application are solved.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a method for preparing high-purity desloratadine. Background technique [0002] Desloratadine, chemically known as 8-chloro-6,11-dihydro-11(4-piperidinylidene)-5H-benzo-5,6-heptane 1,2-b-pyridine, is a non-sedating A long-acting tricyclic antihistamine, which is an active metabolite of loratadine, can relieve symptoms related to allergic rhinitis or chronic idiopathic urticaria by selectively antagonizing peripheral H1 receptors. Compared with the first-generation and second-generation antihistamines, desloratadine has the advantages of strong effect, fast onset, long duration of action, and low toxicity. Current studies have confirmed that desloratadine can improve allergic reactions. It is superior to loratadine and other antihistamines in terms of rhinitis and nasal congestion symptoms, and has a decongestant-like effect. [0003] Since desloratadine i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 管小明刘铁薇韩玉呈汪勇杨东雄
Owner GUANGDONG JIUMING PHARMA
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