A kind of preparation method of medicinal scopolamine butylbromide

A technology of scopolamine and scopolamine, which is applied in the field of preparation of medicinal scopolamine butylbromide, can solve the problems of difficult post-processing, low yield, and the quality of finished products cannot meet the European Pharmacopoeia, and achieves less raw material residues, high yield, The effect of shortening the processing time

Active Publication Date: 2021-03-23
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Because there is low yield in the prior art, post-processing difficulty is big, and finished product quality does not reach defectives such as European Pharmacopoeia, therefore will develop a kind of yield height, and post-processing is simple, and finished product quality meets the preparation of Scopolamine Butylbromide stipulated in European Pharmacopoeia and its preparation method. Purification process

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  • A kind of preparation method of medicinal scopolamine butylbromide
  • A kind of preparation method of medicinal scopolamine butylbromide

Examples

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Embodiment 1

[0028] An embodiment of the preparation method of the pharmaceutical butterchromatic alkalikine of the present invention, including the following steps:

[0029] (1) Preparation of buddus of butchromonoli: 5 g of Eastern alkali is dissolved in 2.5 ml of bromo n-butyl, then 1 ml of acetonitrile, heating at 65 ° C for 60 h; after the reaction is completed, the volume fraction of Eastern alkali weight is 0.5 times volume is 70%. Ethanol solution is concentrated under reduced pressure, and there is a crude bromide of butterolactone;

[0030] (2) Purification: The above-mentioned butchromodide is added to a methanol solution of 70%, after dissolving, filtration, placing room temperature, precipitated crystals in the refrigerator for 4 h, filtration, wash, and then dried The above operation was repeated, and the second, three, four-time recrystallization was carried out, and the drug was carried out at 70 ° C for 16 h at 70 ° C, i.e..

[0031] After testing, the product was 5.5 g, the y...

Embodiment 2

[0033] An embodiment of the preparation method of the pharmaceutical butterchromatic alkalikine of the present invention, including the following steps:

[0034] (1) Preparation of birundine of butchromoni: 5 g of Eastern alkali is dissolved in 7.5 ml of bromine n-butylation, then 10 ml of pyridine, heating at 80 ° C for 20 h; the reaction is completed, and the amount of anhydrous alkali is 5 times the volume of anhydrous ethanol is concentrated. , Deboratomodorine crude;

[0035] (2) Purification: The above-mentioned butchromodide is added to 25 ml of anhydrous methanol. After dissolving, it is filtered through heat, placed at room temperature, and precipitated crystals and placed in the refrigerator for 4 h, then dried at 100 ° C for 5 h, Medicine butterromide.

[0036] It was detected, and the product was 6 g, the yield was 120%, and the purity was 99.6%. Eastern is 0.07% of the bloodstatal mass, and other single maximum hetero mass of 0.16%, and the content is 99.6%.

Embodiment 3

[0038] An embodiment of the preparation method of the pharmaceutical butterchromatic alkalikine of the present invention, including the following steps:

[0039] (1) Preparation of birrochlorine alkaline: 20 g of east alkali is dissolved in 30 ml of bromine n-butyne, then 20 mL of acetonitrile, heating at 80 ° C for 35 h; the reaction ends, the volume fraction of the eastiorine base is 90% methanol The solution was concentrated under reduced pressure, and there was a crude bromoantine.

[0040] (2) Purification: The above-mentioned butchromodiochioline is added to the ethanol solution of 40 ml of volume fraction. After dissolving, it is filtered through heat, placed at room temperature, precipitated crystals in the refrigerator for 4 h, filtered, wash and dried The above operation was repeated in the addition of 75% of the ethanol solution, and the second recrystallization was performed, and the drug was dried in vacuo to dry at 100 ° C, i.e.

[0041] After testing, 23.6 g of the ...

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Abstract

The invention discloses a medical scopolamine butylbromide preparation method which comprises the following steps: (1) scopolamine butylbromide crude product preparation: evenly mixing scopolamine, butyl bromide and a solvent A, performing heating and refluxing reaction and adding a solvent B to perform vacuum concentration after reaction to obtain a scopolamine butylbromide crude product; (2) purification: recrystallizing the scopolamine butylbromide crude product by a solvent C and vacuum drying to obtain medical scopolamine butylbromide. The scopolamine butylbromide preparation method disclosed by the invention has the advantages of convenience in technological operation, high yield, low cost, high product purity, easiness in industrialized production and the like.

Description

Technical field [0001] The present invention belongs to the field of chemical synthesis, and more particularly to a method of preparing a pharmaceutical butbondromide. Background technique [0002] Dobromomide is a choline receptor block, which is chemically called: bromination 6β, 7β-epoxy-3α-hydroxy-8-butyl-Lα-H, 5αH-vikane (-)-Trust The serial acid ester. Molecular formula: c 21 Hide 30 BRNO 4 . 1950 was developed by Boehringer, Germany, and the commodity names were Buscopan. The butterromonium alkali has a smooth muscle, and it is also possible to inhibit the conduction of the ganglium, acting on the sub-intersectional nervous system, is a drug for treating abdominal colic, esophageal, and kidney colic. [0003] The synthesis method of tanopromonol is mainly used in the literature: (1) method is refluxed by acetonitrile into a medium, and the earthenkine and bromine n-butane 65 ° C is refluxed for 160 hours, and the yield is 65%; (2) method is an easter base and bromine The n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 傅玉萍李文彬唐顺之关伟键许文东袁诚王国财牟肖男江程熊淑娴李咏华王小妹
Owner GUANGZHOU HANFANG PHARMA
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