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Preparation method of flupirtine maleate

A technology of flupirtine maleate and clopyridine, which is applied in the field of preparation of flupirtine maleate, and can solve problems such as no optimization of industrialized large-scale production

Inactive Publication Date: 2012-12-26
SUZHOU ERYE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Chinese Patent Application Publication No. CN102241626A and CN102260209A all disclose the preparation method of flupirtine maleate, but the preparation method in these two applications is all laboratory Scale, not optimized for industrial mass production

Method used

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  • Preparation method of flupirtine maleate
  • Preparation method of flupirtine maleate
  • Preparation method of flupirtine maleate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0095] Embodiment 1——Preparation experiment of flupirtine maleate

[0096] (1) Substitution reaction - synthesis of intermediate F1

[0097] I. Feeding amount and ratio

[0098] name kg mol 2-Amino-3-nitro-6-chloropyridine 5.0 28.9 Absolute ethanol 14.0 -- p-Fluorobenzylamine 4.3 34.4 Sodium carbonate 6.02 -- pyridine 0.85 -- purified water 34.0 --

[0099] II. Experimental process

[0100] Put 2-amino-3-nitro-6-chloropyridine, sodium carbonate, absolute ethanol, and pyridine into a dry 211# reactor, start stirring and heat to about 80°C (80°C±5°C), Obvious reflux; slowly drop p-fluorobenzylamine into the reaction kettle, after the dropwise addition, stir and reflux at about 80°C (80°C±5°C) for about 4 hours.

[0101] Stop heating, add 34.0kg of purified water, stir and cool down to room temperature (25°C±5°C), a large amount of yellow crystals precipitated.

[0102] Filter, collect the filter cake, wash the filte...

Embodiment 2

[0141] Embodiment 2 - the control of key steps and the refinement of product

[0142] The production of this product is divided into five steps: substitution reaction, reduction reaction, acylation reaction, salt formation, and refining. Among them, the substitution reaction can obtain solid products, and the products of reduction reaction and acylation reaction are not easy to obtain solids during operation, and the products are easy to produce. The crude product obtained by oxidation and salt formation is not easy to be refined after drying, and the small amount of water contained in the crude product has no obvious influence on the quality of the finished product. During the experiment, we focused on the reaction temperature, material feeding ratio, and reaction time as the research objects, and gradually explored the corresponding parameters.

[0143]

[0144] In the synthesis process, the product of the substitution reaction is the intermediate F1 and can be separated...

Embodiment 3

[0150] Embodiment 3——Multi-batch process research and data summary thereof

[0151] According to the above-mentioned preparation method of flupirtine maleate, multiple batches and different batch sizes of trial production were carried out, and the yield and product quality were studied, and the data are shown in the table below. The data show that the synthetic method of the present invention is stable and reliable, can obtain high-purity products, and at the same time, the content of related substances and the largest single impurity is very low, the process parameters are stable, the reproducibility is good, and the product quality is stable.

[0152]

[0153]

[0154]

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Abstract

The invention provides a novel preparation method of flupirtine maleate; the method mainly comprises steps of substitution reaction, reduction reaction, acylation reaction, salt forming reaction and refining. It is proved by small and medium scale tests that a novel process route and reaction process are achievable, technical parameters are stable, reproducibility is good and product quality is stable.

Description

technical field [0001] The invention belongs to the technical field of chemical medicine preparation. Specifically, the present invention relates to a preparation method of flupirtine maleate. Background technique [0002] Flupirtine maleate is a non-opioid analgesic that acts on the central nervous system. Neuroprotective triple action. It is mainly used for the treatment of various types of moderate acute pain, such as pain caused by surgery, trauma, etc., as well as headache / migraine and abdominal cramps. [0003] The English name of flupirtine maleate is: Flupirtine Maleate, chemical name: ethyl 2-amino-6-[((4-fluorophenyl)methyl)amino]pyridine-3-carbamate maleate; Chemical Abstracts (CAS) number: 75507-68-5; Molecular formula: C 15 h 17 FN 4 o 2 ·C 4 h 4 o 4 ; Molecular weight: 420.39; Its structural formula is: . [0004] From the structural point of view, flupirtine maleate is a molecular compound, and flupirtine is synthesized from benzene derivatives ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/75
Inventor 时明生陈学文陆夕明刘志朱炜
Owner SUZHOU ERYE PHARMA CO LTD
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