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Medical scopolamine butylbromide preparation method

A technology of scopolamine and scopolamine, which is applied in the field of preparation of medicinal scopolamine butylbromide, can solve the problems of low yield, the quality of the finished product cannot meet the European Pharmacopoeia, and the difficulty of post-processing, so as to achieve high yield and shorten the processing time , The effect of less raw material residue

Active Publication Date: 2018-12-21
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

Method used

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  • Medical scopolamine butylbromide preparation method
  • Medical scopolamine butylbromide preparation method

Examples

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Embodiment 1

[0028] A kind of embodiment of the preparation method of medicinal scopolamine butylbromide of the present invention comprises the following steps:

[0029] (1) Preparation of butyl bromide scopolamine crude product: Dissolve 5 g scopolamine in 2.5 ml n-bromobutane, then add 1 ml acetonitrile, heat and react at 65° C. for 60 h; after the reaction, add 0.5 times the volume of scopolamine weight to make the volume fraction 70% The ethanol solution was concentrated under reduced pressure to obtain the crude product of scopolamine butylbromide;

[0030] (2) Purification: Add the above-mentioned scopolamine butylbromide crude product into 6ml of methanol solution with a volume fraction of 70%. After the dissolution is complete, filter it while it is hot, place it at room temperature, and place it in the refrigerator for 4 hours after the crystals are precipitated, filter it, wash it and drain it, and then Add 6ml of methanol solution with a volume fraction of 70% to repeat the abov...

Embodiment 2

[0033] A kind of embodiment of the preparation method of medicinal scopolamine butylbromide of the present invention comprises the following steps:

[0034] (1) Preparation of crude scopolamine butyl bromide: Dissolve 5 g of scopolamine in 7.5 ml of n-butane bromide, then add 10 ml of pyridine, heat and react at 80° C. for 20 h; after the reaction is completed, add dehydrated alcohol with 5 times the volume of scopolamine weight and concentrate under reduced pressure , to obtain the crude product of scopolamine butylbromide;

[0035] (2) Purification: Add 25ml of anhydrous methanol to the crude product of scopolamine butylbromide, and after the dissolution is complete, filter it while it is hot, place it at room temperature, place it in the refrigerator for 4 hours after the crystals are precipitated, and then dry it in vacuum at 100°C for 5 hours to obtain the Scopolamine Butylbromide.

[0036] After testing, 6g of the finished product was obtained, with a yield of 120% and ...

Embodiment 3

[0038] A kind of embodiment of the preparation method of medicinal scopolamine butylbromide of the present invention comprises the following steps:

[0039] (1) Preparation of butyl bromide scopolamine crude product: 20 g scopolamine is dissolved in 30 ml n-bromobutane, then 20 ml acetonitrile is added, and the reaction is heated at 80° C. for 35 h; the reaction is completed, and the volume fraction of scopolamine 3 times the volume is 90% methanol The solution was concentrated under reduced pressure to obtain the crude product of scopolamine butylbromide;

[0040] (2) Purification: add the above-mentioned scopolamine butyl bromide crude product into 40ml of ethanol solution with a volume fraction of 75%, after the dissolution is complete, filter while it is hot, place it at room temperature, place it in the refrigerator for 4 hours after the crystals are precipitated, filter, wash and drain, and then Add 30ml of ethanol solution with a volume fraction of 75% to repeat the abo...

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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 invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of medicinal scopolamine butylbromide. Background technique [0002] Scopolamine butylbromide is a cholinergic receptor blocker, its chemical name is: bromide 6β, 7β-epoxy-3α-hydroxy-8-butyl-lα-H, 5αH-tropane(-)-trop Pinate. Molecular formula: C 21 h 30 BrNO 4 . Developed by the German Boehringer company in 1950, the trade name is Buscopan. Scopolamine butylbromide not only has antispasmodic effect on smooth muscle, but also inhibits the conduction of ganglion, acts on the parasympathetic nervous system, and is a drug used to treat abdominal colic, esophageal spasm and renal colic. [0003] The synthetic method of Scopolamine butylbromide of bibliographical information mainly contains following two kinds: (1) method is medium with acetonitrile, 65 ℃ of reflux reactions of scopolamine and n-butane bromide 160 hours, yield 65%; (2) ...

Claims

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Application Information

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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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