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A kind of purification production method of Pisicarib hydrochloride

A technology for the production of Piscicarbyl Hydrochloride and its production method, which is applied in the field of purification of Piscicarbyl Hydrochloride, which can solve the problems of potential safety hazards of purified products, and achieve the effects of being convenient for industrial production, less times of purification, and simple in the operation process

Active Publication Date: 2016-04-27
BEIJING JIALIN PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With this system, the purity can only reach 98.5% at one time, and multiple purifications are required. In addition, because ether is used in the purification process, there is a small amount of peroxide in the ether, which makes the purified product have a greater safety hazard during the vacuum drying process.

Method used

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  • A kind of purification production method of Pisicarib hydrochloride
  • A kind of purification production method of Pisicarib hydrochloride
  • A kind of purification production method of Pisicarib hydrochloride

Examples

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Effect test

Embodiment 1

[0037] Embodiment 1. the purification of Pixicaride Hydrochloride

[0038] In a 250ml three-necked flask, add 53g of crude product of Pisicani hydrochloride (prepared according to the crude product of Pisicani hydrochloride), 160ml of N,N-dimethylformamide, stir and heat until completely dissolved, add 2.7g of activated carbon and heat to 130 After decolorizing at ℃ for 1 hour, lower the temperature to 80℃ and filter while hot to obtain the mother liquor. The mother liquor was naturally stirred and cooled to room temperature, and a large amount of off-white precipitate was precipitated. Filtered and dried to obtain a light white solid, wet weight: 48g. After natural air drying, vacuum drying at 60° C. for 10 hours gave 45 g of solid, yield: 84.9%. HPLC: 99.99%, the single largest impurity is less than 0.1%, see HPLC spectrum figure 2 .

[0039] 1 H-NMR (CDCl 3 δppm) 2.014 (m, 4H), 2.168 (t, 2H), 2.23 (s, 6H), 2.56 (m, 2H), 2.89 (d, 2H), 3.03 (s, 1H), 3.33 (2, 2H) , 3.78 ...

Embodiment 2

[0040] Embodiment 2. Purification of Pisicarib Hydrochloride

[0041] In a 250ml three-necked flask, add 53g of crude product of Piscicanide Hydrochloride (prepared according to the crude product of Piscicarnate Hydrochloride), 160ml of N,N-dimethylacetamide, stir and heat until completely dissolved, add 2.7g of activated carbon and heat to 130 After decolorizing at ℃ for 1 hour, lower the temperature to 80℃ and filter while it is hot to obtain the mother liquor. The mother liquor is naturally stirred and cooled to room temperature, and a large amount of off-white precipitate precipitates. Filter and drain to obtain a light white solid, wet weight: 47g. After natural air drying, vacuum drying at 60° C. for 10 hours gave 45.2 g of solid, yield: 85.2%. HPLC: 99.97%, the single largest impurity is less than 0.1%. See HPLC chromatogram Figure 4 .

Embodiment 3

[0042] Example 3. Purification of Pisicarib Hydrochloride

[0043]In a 250ml three-neck flask, add 53g of crude product of Piscicanide Hydrochloride (prepared according to the crude product of Piscicanide Hydrochloride), 160ml of N,N-diethylformamide, stir and heat until completely dissolved, add 2.7g of activated carbon and heat to 130 After decolorizing at ℃ for 1 hour, lower the temperature to 80℃ and filter while it is hot to obtain the mother liquor. The mother liquor is naturally stirred and cooled to room temperature, and a large amount of off-white precipitate precipitates. Filter and drain to obtain a light white solid, wet weight: 47g. After natural air drying, vacuum drying at 60° C. for 10 hours gave 40 g of solid, yield: 68.4 g%. HPLC: 99.96%, the single largest impurity is less than 0.1%. See HPLC chromatogram Figure 5 .

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Abstract

The invention discloses a purification production method of pilsicainide hydrochloride. A high-purity pilsicainide hydrochloride product can be obtained by purifying a pilsicainide hydrochloride crude product through procedures of thermal dissolving by using an amine solvent, decoloring by using activated carbon, thermal filtering, cold separation and the like. The method is economic and practical and easy for industrial production.

Description

technical field [0001] The present invention relates to a kind of purification production method of Pixicaride hydrochloride. Background technique [0002] Pilsicainide Hydrochloride, the English name is Pilsicainide Hydrochloride, its chemical structure is as follows: [0003] [0004] Pisicarib hydrochloride is a Na channel blocker developed by Suntory Corporation of Japan (now Daiichi Pharmaceutical Co., Ltd.). It belongs to class Ic antiarrhythmic drugs and is used for the treatment of supraventricular arrhythmias. Clinical trials have shown that this product can significantly improve supraventricular premature beats, premature ventricular beats, paroxysmal ventricular tachycardia, paroxysmal atrial fibrillation, and atrial flutter. There are no common side effects of other arrhythmia drugs. [0005] There are two methods for the synthesis of picicanilide hydrochloride (1) Δ 1,(8) -Dehydrodicondensed pyrrolidine reacts with malonic acid to obtain tetrahydrodiconden...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 高传夫张晓峰李振洁田凤鸣张维伟高洪敏王士辉杨爽
Owner BEIJING JIALIN PHARM INC
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