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Novel chlortrimeton impurity and preparation process thereof

A technology for chlorpheniramine and impurities, which is applied in the field of new chlorpheniramine impurities and its preparation, can solve problems such as difficult separation and achieve good application prospects

Pending Publication Date: 2020-05-05
CHENGDU JIANJIANG PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The inventor has found through research that there is generally an impurity in the finished product of chlorpheniramine maleate, which has a structure close to that of chlorpheniramine maleate and is difficult to separate

Method used

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  • Novel chlortrimeton impurity and preparation process thereof
  • Novel chlortrimeton impurity and preparation process thereof
  • Novel chlortrimeton impurity and preparation process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1, the preparation of chlorpheniramine impurity of the present invention

[0047]

[0048] (1) Preparation of compound 2:

[0049] 200g of p-chlorophenylacetonitrile, 100g of 2-chloropyridine, and 600ml of toluene were added to the reaction flask, cooled to 15°C in ice water, and 51.5g of sodium amide was added. After the addition was completed, the reaction was carried out at room temperature for 2-5 hours, and the reaction was completed by TLC monitoring. The reaction solution was quenched by adding water, the aqueous layer was separated, the organic layer was washed with 200 ml of brine, and the organic phase was concentrated to obtain 190 g of compound 1 as an oil, with a yield of 95%.

[0050] Then add compound 1 (11.5g) into a 150ml single-necked bottle, add 50ml of toluene to dissolve, then slowly add 6.8g of sodium ethoxide, after dissolving, add 0.1g of tetrabutylammonium bromide, heat up to 35°C, add bromoacetaldehyde dropwise A solution of diet...

experiment example 1

[0055] Experimental example 1, the effect of chlorpheniramine impurity of the present invention in the quality detection of chlorpheniramine test article as positive control substance

[0056] 1. Experimental method

[0057] According to the high performance liquid phase method (general rule 0512), measure the content of chlorpheniramine maleate impurity in the test solution of chlorpheniramine maleate. Among them, chlorpheniramine maleate is a commercially available product or prepared according to a known method (such as the method described in patent application 201910251936.4).

[0058] Chromatographic conditions: Octadecylsilane bonded silica gel is used as filler, and the chromatographic column is Ultimate XDB-C18 (4.6*300mm, 5μm); 8.57g / L NH 4 h 2 PO 4 (adjust pH 3.0 with phosphoric acid)-acetonitrile (80:20) as mobile phase; detection wavelength 225nm; flow rate 1.0ml / min; column temperature 35°C.

[0059] Reference substance solution: accurately take the chlorphenir...

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Abstract

The invention provides a chlortrimeton impurity. The structure of the chlortrimeton impurity is shown in the specification. The invention also provides a preparation process of the chlortrimeton impurity. Experiments prove that the chlortrimeton impurity exists in finished products of chlorpheniramine maleate, and the structure of the chlortrimeton impurity is close to that of chlorpheniramine maleate, so that the separation difficulty is high. However, the chlortrimeton impurity is prepared by a simple process, can be used as a reference substance for quality control of chlorpheniramine maleate, and has a very good application prospect.

Description

technical field [0001] The invention belongs to the field of medicine purification, and in particular relates to a new chlorpheniramine impurity and a preparation process thereof. Background technique [0002] Chlorpheniramine maleate, also known as chlorpheniramine, chlorpheniramine, malealamine, chlortrimidone. It is an antihistamine drug, which can play an anti-allergic effect by antagonizing the H1 receptor. It is mainly used for rhinitis, skin and mucous membrane allergies, and relief of cold symptoms such as tearing, sneezing, and runny nose. The structural formula is as follows: [0003] [0004] The inventor found through research that an impurity generally exists in the finished product of chlorpheniramine maleate, and the structure of this impurity is close to that of chlorpheniramine maleate, and the separation is difficult. Therefore, if can find a kind of simple method to prepare the pure product of this impurity, just can use it as reference substance to ...

Claims

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Application Information

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IPC IPC(8): C07D213/57G01N30/02G01N30/06
CPCC07D213/57G01N30/02G01N30/06G01N2030/062
Inventor 黄忠超张强吴金伟
Owner CHENGDU JIANJIANG PHARMA FACTORY
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