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A kind of refining method of methyl bromide homatropine

A technology of homatropine bromide and its refining method is applied in the field of homatropine bromide purification to achieve the effects of simple operation and mild reaction conditions

Active Publication Date: 2018-01-12
HUBEI BIOCAUSE HEILEN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are no documents and patents related to the refining method of methyl bromide homatropine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 100g of the crude methyl bromide homatropine (purity 98.2%), add it to 150g of ethanol, heat up to 75°C to dissolve, continue to stir for about 20min, at room temperature, gradually add the above solution into 1000g of acetone and stir, then cool down to 0 Crystallize at about ℃, grow crystal for 2 hours. Suction filtration, vacuum drying at 60°C for 7 hours to obtain 75.6 g of methyl bromide homatropine fine product.

Embodiment 2

[0020] Take 100g of the crude methyl bromide homatropine (purity 98.2%), add it to 100g of methanol, heat up to 60°C to dissolve, continue to stir for about 20min, at room temperature, gradually add the above solution into 800g of acetone and stir, then cool down to 0 Crystallize at about ℃, grow crystal for 2 hours. Suction filtration, vacuum drying at 60°C for 5 hours to obtain 72.3 g of methyl bromide homatropine fine product.

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Abstract

The invention relates to a refining method of homatropine methylbromide. The refining method mainly comprises the following steps of dissolving homatropine methylbromide into an organic solvent A, heating, adding into an organic solvent B, cooling, and crystallizing. The refining method has the advantages that the purity of the homatropine methylbromide reaches not less than 99.5%, the CP\USP\EP (Chinese Pharmacopoeia\The United States Pharmacopeia\European Pharmacopeia) standard is met, the reaction condition is moderate, the operation is simple and convenient, and the refining method is suitable for industrialized production.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a method for refining homatropine bromide. Background technique [0002] At present, Homatropine bromide, also known as Homatropine bromide, has an English name of Homatropine Methylbromide. It has the effect of blocking acetylcholine, causing pupillary sphincter and cycloparalysis, causing mydriasis and regulating paralysis. Its ability to block cholinergic nerves is faster and weaker than atropine. The duration of its mydriasis and regulation of paralysis is much shorter than that of atropine, and its adverse reactions are mild, without the side effect of inhibiting secretion and making the throat feel dry. Therefore, it is more convenient for mydriasis to check the fundus and optometry. There are not many documents about the preparation method of bromide homatropine, and the related documents are: "research and industry, 1972, 17 (3), 92-93" prepared by the reaction process of tropi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 刘寒星谢三龙石秀兰刘润涛
Owner HUBEI BIOCAUSE HEILEN PHARM CO LTD