Detection method of (6-aminopyridine-2-yl)(1-methylpiperidine-4-yl) ketone dihydrochloride

A technology of methylpiperidine and aminopyridine is applied in the detection field of ketone dihydrochloride, which can solve the problem of not finding a purity detection method, and achieve the effects of improving separation effect, good repeatability and improving detection accuracy.

Active Publication Date: 2021-12-31
FOSHAN ENANTIOSIC CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are no related documents and reports on the purity detection method of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride. -2-base) the quality control of (1-methylpiperidin-4-yl) ketone dihydrochloride, further control the quality of lasmidiptan, provide a kind of (6-aminopyridin-2-yl) The detection method of the purity and impurity content of (1-methylpiperidin-4-yl)methanone dihydrochloride is particularly important

Method used

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  • Detection method of (6-aminopyridine-2-yl)(1-methylpiperidine-4-yl) ketone dihydrochloride
  • Detection method of (6-aminopyridine-2-yl)(1-methylpiperidine-4-yl) ketone dihydrochloride
  • Detection method of (6-aminopyridine-2-yl)(1-methylpiperidine-4-yl) ketone dihydrochloride

Examples

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Embodiment 1

[0063] A detection method of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride, comprising the steps:

[0064] 1) Reference substance solution preparation: take an appropriate amount of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride reference substance, and use 50% volume percent concentration Acetonitrile aqueous solution was dissolved to obtain a reference substance solution with a concentration of 0.5 mg / mL;

[0065] 2) Preparation of the test solution: take an appropriate amount of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride for the test, and use a volume percent concentration of 50 % acetonitrile aqueous solution was dissolved to obtain a concentration of 0.5mg / mL reference substance solution;

[0066] 3) System suitability solution preparation: take an appropriate amount of (6-aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone dihydrochloride reference substance, (6-bromo-2-pyridine Base) (1-methyl-4...

Embodiment 2

[0096] A detection method of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride, comprising the steps:

[0097] 1) Reference substance solution preparation: take an appropriate amount of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride reference substance, and use 50% volume percent concentration Acetonitrile aqueous solution was dissolved to obtain a reference substance solution with a concentration of 0.5 mg / mL;

[0098] 2) Preparation of the test solution: take an appropriate amount of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride for the test, and use a volume percent concentration of 50 % acetonitrile aqueous solution was dissolved to obtain a concentration of 0.5mg / mL reference substance solution;

[0099] 3) System suitability solution preparation: take an appropriate amount of (6-aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone dihydrochloride reference substance, (6-bromo-2-pyridine Base) (1-methyl-4...

Embodiment 3

[0113] A detection method of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride, comprising the steps:

[0114] 1) Reference substance solution preparation: take an appropriate amount of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride reference substance, and use 50% volume percent concentration Acetonitrile aqueous solution was dissolved to obtain a reference substance solution with a concentration of 0.5 mg / mL;

[0115] 2) Preparation of the test solution: take an appropriate amount of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride for the test, and use a volume percent concentration of 50 % acetonitrile aqueous solution was dissolved to obtain a concentration of 0.5mg / mL reference substance solution;

[0116] 3) System suitability solution preparation: take an appropriate amount of (6-aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone dihydrochloride reference substance, (6-bromo-2-pyridine Base) (1-methyl-4...

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Abstract

The invention belongs to the technical field of organic matter detection and analysis, and discloses a detection method of (6-aminopyridine-2-yl)(1-methylpiperidine-4-yl) ketone dihydrochloride. The detection method comprises the following steps: detecting (6-aminopyridine-2-yl) (1-methylpiperidine-4-yl) ketone dihydrochloride by adopting a liquid chromatography method, wherein the conditions of the liquid chromatography are as follows: the adopted mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is a phosphate buffer solution, the mobile phase B is acetonitrile, and the mobile phase is subjected to gradient elution according to certain conditions. The detection method can be used for accurately detecting the purity of the (6-aminopyridine-2-yl)(1-methylpiperidine-4-yl) ketone dihydrochloride in the test sample.

Description

technical field [0001] The invention belongs to the technical field of organic matter detection and analysis, in particular to a detection method of (6-aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone dihydrochloride. Background technique [0002] (6-Aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone dihydrochloride, CAS number: 613678-10-7, this compound is an important compound for the production of the drug Lasmidiptan The purity and impurities of intermediates directly affect the purity of the drug and the size of the impurities, thus directly affecting the curative effect of the drug. [0003] At present, there are no related documents and reports on the purity detection method of (6-aminopyridin-2-yl) (1-methylpiperidin-4-yl) ketone dihydrochloride. -2-base) the quality control of (1-methylpiperidin-4-yl) ketone dihydrochloride, further control the quality of lasmidiptan, provide a kind of (6-aminopyridin-2-yl) The detection method of the purity and impurity cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/74Y02P20/55
Inventor 卢彪邓伟梁徐亮周炳乾黄晓韵陈昌龙徐剑黄志豪蔡祥
Owner FOSHAN ENANTIOSIC CORP LTD
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