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Separation and detection method of 3-chloro-4-methoxybenzylamine hydrochloride isomer

A technology of methoxybenzylamine hydrochloride and isomers, which is applied in the field of separation of 3-chloro-4-methoxybenzylamine hydrochloride isomers, and can solve the problem of affecting the quality of final products and other problems, to achieve the effect of efficient and rapid separation and improvement of purity

Inactive Publication Date: 2018-09-28
无锡富泽药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 4-(3-Chloro-4-methoxybenzylamino)5-ethoxycarbonyl-2-methylthiopyrimidine is an important starting material for the synthesis of avanafil, while 3-chloro-4-methoxy Benzylbenzylamine hydrochloride (hereinafter referred to as raw material 1) is an important raw material for the synthesis of (3-chloro-4-methoxybenzylamino) 5-ethoxycarbonyl-2-methylthiopyrimidine, if it contains isomer Body 2-chloro-4-methoxybenzylamine hydrochloride (hereinafter referred to as impurity 1), will produce a series of impurities in the reaction, affecting the quality of the final product

Method used

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  • Separation and detection method of 3-chloro-4-methoxybenzylamine hydrochloride isomer
  • Separation and detection method of 3-chloro-4-methoxybenzylamine hydrochloride isomer
  • Separation and detection method of 3-chloro-4-methoxybenzylamine hydrochloride isomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Detection conditions:

[0028] Instrument: Agilent 1100 high performance liquid chromatography, detection wavelength is 230nm.

[0029] The capillary column model is Inertsil ODS-3, the size of the capillary column is 4.6×250mm×5 μm, the octadecylsilane-bonded silica gel filler is used as the stationary phase, and acetonitrile-0.02mol / L sodium dihydrogen phosphate solution is used as the mobile phase.

[0030] Solvent: The volume ratio of phase A to phase B is 55:45.

[0031] Mobile phase: A is 0.02mol / L sodium dihydrogen phosphate solution, phase B is acetonitrile, isocratic elution, the volume ratio of phase A to phase B is 90:10.

[0032] Flow rate: 0.9ml / min.

[0033] Column temperature: 35°C.

[0034] Injection volume: 5 μL.

[0035] Running time: 20min;

[0036] Detection steps: take the mixed solution of the above-mentioned raw material 1 and impurity 1, carry out high-performance liquid chromatography analysis according to the above-mentioned conditions, re...

Embodiment 2

[0039] Detection conditions:

[0040] Instrument: Agilent 1100 high performance liquid chromatography, detection wavelength is 230nm.

[0041] The capillary column model is Inertsil ODS-3, the size of the capillary column is 4.6×250mm×5 μm, the octadecylsilane-bonded silica gel filler is used as the stationary phase, and acetonitrile-0.02mol / L sodium dihydrogen phosphate solution is used as the mobile phase.

[0042] Solvent: The volume ratio of phase A to phase B is 55:45.

[0043] Mobile phase: A is 0.02mol / L sodium dihydrogen phosphate solution, phase B is acetonitrile, isocratic elution, the volume ratio of phase A to phase B is 85:15.

[0044] Flow rate: 1.0ml / min.

[0045] Column temperature: 35°C.

[0046] Injection volume: 8 μL.

[0047] Running time: 20min.

[0048] Detection steps: take the mixed solution of the above-mentioned raw material 1 and impurity 1, carry out high-performance liquid chromatography analysis according to the above-mentioned conditions, re...

Embodiment 3

[0051] Detection conditions:

[0052] Instrument: Agilent 1100 high performance liquid chromatography, detection wavelength is 230nm.

[0053]The capillary column model is Inertsil ODS-3, the size of the capillary column is 4.6×250mm×5 μm, the octadecylsilane-bonded silica gel filler is used as the stationary phase, and acetonitrile-0.02mol / L sodium dihydrogen phosphate solution is used as the mobile phase.

[0054] Solvent: The volume ratio of phase A to phase B is 55:45.

[0055] Mobile phase: A is 0.02mol / L sodium dihydrogen phosphate solution, phase B is acetonitrile, isocratic elution, the volume ratio of phase A to phase B is 80:20.

[0056] Flow rate: 1.1ml / min.

[0057] Column temperature: 35°C.

[0058] Injection volume: 10 μL.

[0059] Running time: 20min.

[0060] Detection steps: take the mixed solution of the above-mentioned raw material 1 and impurity 1, carry out high-performance liquid chromatography analysis according to the above-mentioned conditions, re...

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Abstract

The invention provides the separation and detection method of 3-chloro-4-methoxybenzylamine hydrochloride isomer. The separation method comprises the following steps: taking octadecylsilane-bonded silica gel filler as the fixed phase, taking acetonitrile- 0.02 mol / L sodium dihydrogen phosphate solution as the mobile phase in an efficient liquid chromatograph, adopting high performance liquid chromatography to make direct resolution, the volume ratio of the acetonitrile in the acetonitrile 0.02 mol / L sodium dihydrogen phosphate solution was 10%-20%. The separation and detection method of 3-chloro-4-methoxybenzylamine hydrochloride isomer as is disclosed realizes the efficient and rapid separation of the 3-chloro-4-methoxybenzylamine hydrochloride isomer, thereby improving the purity of the3-chloro-4-methoxybenzylamine hydrochloride.

Description

technical field [0001] The invention relates to the technical field of medical detection, in particular to a method for separating and detecting isomers of 3-chloro-4-methoxybenzylamine hydrochloride. Background technique [0002] Avanafil CAS registration number: 330784-47-9, is a drug developed by Vivus Pharmaceutical Company of the United States authorized by Mitsubishi Tanabe Pharmaceutical Co., Ltd. of Japan for the treatment of male erectile dysfunction. On April 27, 2012, it was approved by the US FDA and launched in the United States under the trade name of Stendra. [0003] 4-(3-Chloro-4-methoxybenzylamino)5-ethoxycarbonyl-2-methylthiopyrimidine is an important starting material for the synthesis of avanafil, while 3-chloro-4-methoxy Benzylbenzylamine hydrochloride (hereinafter referred to as raw material 1) is an important raw material for the synthesis of (3-chloro-4-methoxybenzylamino) 5-ethoxycarbonyl-2-methylthiopyrimidine, if it contains isomer Body 2-chloro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 曹敏蔡亮亮谢卫锋吴鹏程李浩源
Owner 无锡富泽药业有限公司