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Novel chlorphenamine maleate oxidation impurity and preparation process thereof

A technology for oxidizing impurities and chlorpheniramine, which is applied in organic chemistry and other fields, can solve the problems of difficult separation and purity, and achieve good application prospects

Pending Publication Date: 2020-04-21
CHENGDU JIANJIANG PHARMA FACTORY
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  • Application Information

AI Technical Summary

Benefits of technology

The technical effect of this patented method involves preparing an intermediate compound called benzene sulfonic acid (BSA) by treating BPA-maleated chlorophenolic ammonium salt solution containing certain chemical groups like phenylthionate or pH sensitive dyes. This intermediate material contains many different types of impurities such as chlorobenzilimide, dichlofenac, pyridazole nitrogen bases, etc., making them challenges when separating these impurity from other components during purification processes used on crude products made up mostly of pure chloroanisorhodiaminetriplets.

Problems solved by technology

This patented technical problem addressed in this patents relates to finding ways to make sure the final product contains only one type of impurities called chiorphenarnimide hydrochlorides (CAS).

Method used

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  • Novel chlorphenamine maleate oxidation impurity and preparation process thereof
  • Novel chlorphenamine maleate oxidation impurity and preparation process thereof
  • Novel chlorphenamine maleate oxidation impurity and preparation process thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1, the preparation of chlorpheniramine oxidation impurity of the present invention

[0033]

[0034] Add 20g of chlorpheniramine and 200ml of dichloromethane into a 500ml single-necked bottle, stir to dissolve, cool down to -10°C, add 14.8g of sodium bicarbonate, add 30.4g of m-chloroperoxybenzoic acid (m-CPBA) in batches, and React at -10°C for 2 hours, TLC monitors the completion of the reaction, add 200ml of water, stir and separate layers, take the organic layer and add 100ml of saturated brine to wash, take the organic layer and add anhydrous sodium sulfate to dry to obtain a crude product. Then take the crude product and pass it through a silica gel column (200-300 mesh silica gel, column length 20cm, eluent is dichloromethane:methanol=10:1v / v) to obtain 15g of the target product (i.e. the oxidized impurity of chlorpheniramine of the present invention). Yield 72.37%, purity 97%.

[0035] Structural characterization of the target product: MS(m / z): 29...

experiment example 1

[0037] Experimental example 1, the effect of chlorpheniramine oxidized impurities of the present invention in the quality detection of chlorpheniramine test product as positive reference substance

[0038] 1. Experimental method

[0039] According to the high performance liquid phase method (general rule 0512), measure the content of chlorpheniramine maleate oxidation impurity in the chlorpheniramine maleate test solution. 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).

[0040] Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel was used as filler, and the chromatographic column was 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. Take 20ul of the s...

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Abstract

The invention provides a chlorphenamine maleate oxidation impurity, which has the structure defined in the specification. The invention also provides a preparation process of the chlorphenamine maleate oxidation impurity. According to the invention, the experiment results prove that the chlorphenamine maleate oxidation impurity generally exists in a chlorphenamine maleate finished product, and thestructure of the chlorphenamine maleate oxidation impurity is close to the structure of chlorphenamine maleate, so that the separation difficulty is relatively high; and the chlorphenamine maleate oxidation impurity is prepared by a simple process, can be used as a reference substance for quality control of chlorphenamine maleate, and has good application prospect.

Description

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Claims

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Application Information

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Owner CHENGDU JIANJIANG PHARMA FACTORY
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