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Method for preparing nicorandil tripolymer

A nicorandil trimer, solid technology, which is applied in the field of preparation of nicorandil trimer, can solve the problem of low yield of nicorandil trimer, difficulty in obtaining, and limitation of nicorandil tripolymer. The research work of polymer impurities and other problems can achieve the effect of rapid acquisition, good purity and high yield.

Active Publication Date: 2019-03-26
燃点(南京)生物医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the acquisition of nicorandil trimer is mainly prepared from the nicorandil reaction solution by preparing the liquid phase. The yield of the prepared nicorandil trimer is low and the acquisition is difficult, which greatly limits the production capacity of nicorandil. The impurity research work of nicorandil trimer, therefore urgently need to find a kind of yield high, the preparation method of nicorandil trimer that is easy to separate

Method used

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  • Method for preparing nicorandil tripolymer
  • Method for preparing nicorandil tripolymer

Examples

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Embodiment 1

[0021] Dissolve Nicorandil (1.0g) in DMA (2mL), stir in an oil bath at 100°C for 4.0h, slowly cool to room temperature, slowly add carbon tetrachloride dropwise, stir and crystallize, a large amount of solids precipitate, filter, The crude product was obtained by washing with tetrahydrofuran, and recrystallized from tetrahydrofuran to obtain 826.2 mg of nicorandil trimer nitrate as a white solid with a purity of 99.89%.

Embodiment 2

[0023] Dissolve Nicorandil (1.0g) in DMA (3mL), stir in an oil bath at 90°C for 5.0h, slowly cool to room temperature, slowly add chloroform dropwise, stir and crystallize, a large amount of solids precipitate out, filter and wash with acetonitrile to obtain The crude product was recrystallized from acetonitrile to obtain 837.4 mg of nicorandil trimer nitrate as a white solid with a purity of 99.91%.

Embodiment 3

[0025] Dissolve Nicorandil (1.0g) in DMF (3mL), stir in an oil bath at 80°C for 6.0h, slowly cool to room temperature, slowly add dichloromethane dropwise, stir and crystallize, a large amount of solid precipitates, filter, and The crude product was obtained by washing with nitrile, and recrystallized from propionitrile to obtain 855.9 mg of nicorandil trimer nitrate as a white solid with a purity of 99.93%.

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Abstract

The invention provides a method for preparing a nicorandil tripolymer. The method comprises the following steps: (1) dissolving nicorandil into an organic solvent, stirring and reacting for 4-7 hours;(2) slowly dropping a crystallization solvent into the reaction solution after the reaction is ended, slowly cooling to a room temperature, stirring and crystallizing, filtering to obtain a crude product, and washing with an organic solvent; and (3) adding the crude product into a re-crystallization solvent, and re-crystallizing, thereby obtaining the solid nicorandil tripolymer nitrate. According to the method for preparing the nicorandil tripolymer disclosed by the invention, the nicorandil tripolymer can be conveniently and rapidly prepared, and the prepared nicorandil tripolymer is high in yield and excellent in purity.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method of a nicorandil trimer. Background technique [0002] Nicorandil (Nicorandil) was developed by Chugai Pharmaceutical Co., Ltd. in Japan and was launched in Japan in 1984. Nicorandil is an antiangina pectoris drug, which belongs to nitrate ester compound. It has the functions of preventing intracellular calcium ion dissociation, increasing the permeability of cell membrane to potassium ion, dilating coronary blood vessels, continuously increasing coronary blood flow, and inhibiting coronary artery spasm. The role of dilating coronary vessels does not affect blood pressure, heart rate, myocardial contractility and myocardial oxygen consumption. Nicorandil also has the effect of inhibiting platelet aggregation and preventing thrombosis. Nicorandil, chemical name: N-(2-hydroxyethyl) nicotinamide nitrate, structural formula: [0003] [0004] The content o...

Claims

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Application Information

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IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 林峰赵维唐亚军吴敏于学珍秦勇胡传良
Owner 燃点(南京)生物医药科技有限公司
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