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Nalmefene hydrochloride purification method

A purification method, the technology of nalmefene, applied in the direction of organic chemistry, etc., can solve problems such as toxicity

Active Publication Date: 2016-11-30
西藏易明西雅医药科技股份有限公司
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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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1: 10 g of crude nalmefene hydrochloride (content 62.3%) was recrystallized with 200 g of ethyl acetate, dried to obtain 5.6 g of pure nalmefene base;

[0024] Step 2: Dissolve 5.6 g of nalmefene base in about 112 g of acetone, filter and add hydrogen chloride ether solution dropwise to pH 2±0.5, filter the solid, wash the solid with acetone first, then wash the solid with anhydrous ether, and dry , to obtain nalmefene hydrochloride crude product 5.35g;

[0025] Step 3: Dissolve the crude nalmefene hydrochloride completely in water at 50°C, heat filter and cool to room temperature, white crystals are precipitated, filter with suction, wash, and dry to obtain 4.8 g of nalmefene hydrochloride.

Embodiment 2

[0027] Step 1: 10 g of crude nalmefene hydrochloride (content 62.3%) was recrystallized with 300 g of ethyl acetate, dried to obtain 6.1 g of pure nalmefene base;

[0028] Step 2: Dissolve nalmefene base in about 150g of acetone, filter and add hydrogen chloride ether solution dropwise to pH 2±0.5, filter the solid, first wash the solid with acetone, then wash the solid with anhydrous ether, and after drying, get Nalmefene hydrochloride crude product 5.85g;

[0029] Step 3: Dissolve the crude nalmefene hydrochloride completely in water at 100°C, heat filter and cool to room temperature, white crystals precipitate, filter with suction, wash, and dry to obtain 5.34 g of nalmefene hydrochloride.

Embodiment 3

[0031] Step 1: 10 g of crude nalmefene hydrochloride (content 62.3%) was recrystallized with 400 g of ethyl acetate, dried to obtain 6.03 g of pure nalmefene base;

[0032] Step 2: Dissolve nalmefene base in about 180g of acetone, filter and add hydrogen chloride ether solution dropwise to pH 2±0.5, filter the solid, first wash the solid with acetone, then wash the solid with anhydrous ether, and after drying, get Nalmefene hydrochloride crude product 5.62g;

[0033] Step 3: Dissolve the crude nalmefene hydrochloride completely in water at 100°C, heat filter and cool to room temperature, white crystals are precipitated, filter with suction, wash, and dry to obtain 5.28 g of nalmefene hydrochloride.

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PUM

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a nalmefene hydrochloride purification method. Nalmefene is used as a raw material, and nalmefene hydrochloride with purity of 99.95% or more is prepared under the action of solvents such as ethyl acetate, acetone and water.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry. It specifically relates to an improved synthesis method of nalmefene. Background technique [0002] Nalmefene, an opiate derivative structurally similar to the opioid antagonist naltrexone, is a known opioid receptor antagonist that inhibits the Pharmacological effects of both agonists produced endogenously in the system. The clinical effectiveness of nalmefene as an antagonist stems from its ability to rapidly and selectively reverse the effects of opioid agonists, including common depression in the central nervous system and respiratory system. [0003] The nalmefene hydrochloride preparation currently on the market is nalmefene hydrochloride injection, and the specification is 1ml: 0.1mg (calculated as nalmefene). Since injections are directly injected into human tissues or blood vessels, the quality of injections must be ensured, among which the quality of raw materials is very...

Claims

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Application Information

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IPC IPC(8): C07D489/08
CPCC07D489/08
Inventor 高帆
Owner 西藏易明西雅医药科技股份有限公司
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