A kind of preparation method of nicorandil dimer

A nicorandil dimer and nicorandil technology are applied in the field of preparation of nicorandil dimer and can solve the problem of low nicorandil dimer yield and limiting nicorandil dimerization The research work of bulk impurities, the difficulty of obtaining and other problems, to achieve the effect of rapid acquisition, good purity and high yield

Active Publication Date: 2022-02-18
BURNING POINT (NANJING) BIOPHARMACEUTICAL TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

Method used

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  • A kind of preparation method of nicorandil dimer
  • A kind of preparation method of nicorandil dimer

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Dissolve Nicorandil (1.0g) in tetrahydrofuran (4mL), stir in an oil bath at 30°C for 6.0h, slowly cool to room temperature, slowly add carbon tetrachloride dropwise, stir and crystallize, a large amount of solids precipitate out, filter, The crude product was obtained by washing with tetrahydrofuran, and recrystallized from tetrahydrofuran to obtain 826.2 mg of nicorandil dimer nitrate as a white solid with a purity of 99.89%.

Embodiment 2

[0023] Dissolve Nicorandil (1.0g) in acetonitrile (5mL), stir in an oil bath at 40°C for 5.0h, slowly cool to room temperature, slowly add chloroform dropwise, stir and crystallize, a large amount of solids precipitate, filter and wash with acetonitrile to obtain The crude product was recrystallized from acetonitrile to obtain 837.4 mg of nicorandil dimer nitrate as a white solid with a purity of 99.91%.

Embodiment 3

[0025] Nicorandil (1.0g) was dissolved in propionitrile (6mL), stirred in an oil bath at 50°C for 4.0h, slowly cooled to room temperature, dichloromethane was slowly added dropwise, stirred and crystallized, a large amount of solids precipitated, filtered, The crude product was obtained by washing with propionitrile, and recrystallized from propionitrile to obtain 855.9 mg of nicorandil dimer nitrate as a white solid with a purity of 99.93%.

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Abstract

The invention provides a preparation method of nicorandil dimer, comprising the following steps: (1) dissolving nicorandil in an organic solvent, stirring and reacting for 2‑6 h; (2) cooling down slowly to Slowly add a crystallization solvent to the reaction solution at room temperature, stir to crystallize, filter to obtain the crude product, and wash with an organic solvent; (3) Add the above crude product to the recrystallization solvent, and after recrystallization, solid Nicorandil is obtained Dimeric nitrate. The preparation method of the nicorandil dimer disclosed by the invention can conveniently and rapidly obtain the nicorandil dimer, and the obtained nicorandil dimer has a high yield and good purity.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method of nicorandil dimer. 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 of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 秦勇赵维唐亚军吴敏于学珍林峰胡传良
Owner BURNING POINT (NANJING) BIOPHARMACEUTICAL TECH CO LTD
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