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Method for preparing high-purity nalmefene hydrochloride

A technology of nalmefene hydrochloride and nalmefene, which is applied in the field of medicine, can solve problems such as toxicity, achieve low cost, simplify the quality inspection process, and ensure safety

Active Publication Date: 2013-04-03
LIAONING HAISCO PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Used chloroform and hexane in this method all belong to the second class solvent of ICH regulation, have certain toxicity, so there is above-mentioned problem equally

Method used

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  • Method for preparing high-purity nalmefene hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 100.0g of crude nalmefene hydrochloride (HPLC content 95.16%) and 400.0ml of distilled water into the three-necked flask, raise the temperature to 85-95°C, and stir to completely dissolve nalmefene hydrochloride. After dissolving, add activated carbon 0.8g, decolorize for 20 minutes, then filter while hot, wash the filter cake with a small amount of hot water, and collect the filtrate. The filtrate was naturally cooled to room temperature, and white crystals were precipitated during the cooling process. The crystallized material was placed in a freezer at 5°C to allow the crystals to fully separate out. After suction filtration, the filter cake was washed with a small amount of cold water and dried at 60°C to obtain 86.3 g of high-purity nalmefene hydrochloride. The HPLC analysis results are shown in Table 1.

Embodiment 2

[0026] Add 100.0g of crude nalmefene hydrochloride (HPLC content 95.16%) and 200.0ml of distilled water into the three-necked flask, raise the temperature to 85-95°C, and stir to completely dissolve nalmefene hydrochloride. After dissolving, add 0.04g of activated carbon, decolorize for 20 minutes, then filter while hot, wash the filter cake with a small amount of hot water, and collect the filtrate. The filtrate was naturally cooled to room temperature, and white crystals were precipitated during the cooling process. The crystallized material was placed in a freezer at 5°C to allow the crystals to fully separate out. After suction filtration, the filter cake was washed with a small amount of cold water and dried at 60°C to obtain 90.5 g of high-purity nalmefene hydrochloride. The HPLC analysis results are shown in Table 1.

Embodiment 3

[0028] Add 100.0g of crude nalmefene hydrochloride (HPLC content 95.16%) and 100.0ml of distilled water into the three-necked flask, raise the temperature to 90-100°C, and stir to completely dissolve nalmefene hydrochloride. After dissolving, add 0.05 g of activated carbon, decolorize for 10 minutes, then filter while hot, wash the filter cake with a small amount of hot water, and collect the filtrate. The filtrate was naturally cooled to room temperature, and white crystals were precipitated during the cooling process. The crystallized material was placed in a freezer at 0°C to allow the crystals to fully separate out. After suction filtration, the filter cake was washed with a small amount of cold water and dried in vacuum at 40°C to obtain 91.8 g of high-purity nalmefene hydrochloride. The HPLC analysis results are shown in Table 1.

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Abstract

The invention relates to a method for preparing high-purity nalmefene hydrochloride, and in particular relates to a method for refining the nalmefene hydrochloride. The method comprises the steps of dissolving a crude product of the nalmefene hydrochloride in right amount of hot water, cooling and separating out the high-purity nalmefene hydrochloride. The method has the following advantages: (1) through refining, the content of the nalmefene hydrochloride is up to more than 99.5%, the content of the maximum single impurity is less than 0.2%, the content of total impurities is less than 0.5% and the prepared nalmefene hydrochloride is excellent in storage stability and suitable for preparing the preparations of parenteral administration; (2) the method is simple in process, simple and convenient for operation and low in cost and suitable for industrial production; and (3) as no organic solvent is used, the damage to operating personnel and environment is avoided, the finished product has no residual organic solvent problem, the quality inspection step is simplified and the medication safety is guaranteed.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of high-purity nalmefene hydrochloride. Background technique [0002] Nalmefene hydrochloride, synthesized in 1975, is another new pure opioid receptor antagonist synthesized after naloxone (NAL) and naltrexone (NTX). It can bind to opioid receptors μ, κ, and δ, and has the strongest binding effect on μ receptors. Nalmefene hydrochloride is a water-soluble derivative of naltrexone, its 6-methylene chemical structure makes it have a long action time, multiple drug routes, high bioavailability, less side effects, stronger physiological activity, and easier penetration Biofilm and other properties have varying degrees of effects on maintaining the normal functions of respiration, circulation, digestion, endocrine and nervous system. Currently, it has been used in the antagonism of narcotic analgesic respiratory depression, the treatment of heart fa...

Claims

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Application Information

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IPC IPC(8): C07D489/08A61K31/485A61K9/08A61P11/00A61P9/04A61P9/00A61P25/32A61P3/04
Inventor 郑伟
Owner LIAONING HAISCO PHARMACEUTICAL CO LTD
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