Palladium removal method for preparation process of tirofiban hydrochloride

A technology of tirofiban and a preparation process is applied in the field of palladium removal of the preparation process of tirofiban hydrochloride, can solve the problems such as no method for removing palladium, excessive metal palladium content, etc., and achieves remarkable effect, simple operation, and reduced Effect of palladium content

Inactive Publication Date: 2019-02-15
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

Both of them used Pd / C as a catalyst in the catalytic hydrogenation reaction, but they did not provide a corresponding method for removing palladium in the post-treatment process, which made the Tirofiban hydrochloride raw drug product have the problem that the metal palladium content exceeded the standard. serious hidden danger

Method used

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  • Palladium removal method for preparation process of tirofiban hydrochloride
  • Palladium removal method for preparation process of tirofiban hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] This embodiment shows the first specific implementation of the palladium removal method of a tirofiban hydrochloride preparation process, which includes the following steps:

[0032] Put 20g of tirofiban hydrochloride into 400ml of methanol solution, which contains 0.001g / ml of triphenylphosphine, keep the temperature at 20°C for 24 hours in a water bath and then filter under reduced pressure, and filter the obtained filter cake with 40ml of methanol After rinsing, it was air-dried at 40°C to obtain 19.55 g of a white solid with a palladium content of 0.7 ppm.

[0033] In the present embodiment, the method for detecting the palladium content of tirofiban hydrochloride is:

[0034] (1) Instruments and reagents

[0035] Instrument: Thermo-Scientific ICE 3500 atomic absorption spectrometer; SOLAAR data workstation V11.03.

[0036] Reagent: palladium standard solution; nitric acid; water is purified water;

[0037] (2) Spectral parameters and atomization conditions

[0...

Embodiment 2

[0053] Put 20 g of tirofiban hydrochloride into 200 ml of ethanol solution of 0.001 g / ml p-methyltriphenylphosphine, keep the temperature at 25° C. in a water bath and stir for 10 h, then filter under reduced pressure, wash the obtained filter cake with 40 ml of methanol, and wash with Air-dried at 40°C to obtain 19.67 g of a white solid with a palladium content of 0.9 ppm.

[0054] For the technical solutions of the same parts in this embodiment and the first embodiment, please refer to the description in the first embodiment, and will not be repeated here.

Embodiment 3

[0056] Put 20g of tirofiban hydrochloride into 600ml of acetonitrile solution of 0.001g / ml tri-n-butylphosphine, keep the temperature at 40°C and stir in a water bath for 30h, then filter under reduced pressure, wash the obtained filter cake with 30ml of methanol, and wash it at 40°C Blast drying gave 19.32 g of a white solid with a palladium content of 0.7 ppm.

[0057] For the technical solutions of the same parts in this embodiment and Embodiment 1 or Embodiment 2, refer to the description in Embodiment 1 or Embodiment 2, and will not be repeated here.

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Abstract

The invention provides a palladium removal method for a preparation process of tirofiban hydrochloride. The method comprises the following steps: N-(butylsulfonyl)-O-[4-(4-piperidynyl)butyl]-L-tyrosine (tirofiban) is added to an organic solution of trialkyl(aryl)phosphine, and the substances are sufficiently stirred and filtered; a filter cake is washed with an organic solvent and dried, and content of remaining palladium is reduced to 1 ppm or lower. Palladium content is reduced for tirofiban hydrochloride prepared with the palladium removal method for the preparation process of tirofiban hydrochloride, and the whole method is simple to operate, has remarkable effect and is applicable to large-scale production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical production and relates to a method for removing palladium in the preparation process of tirofiban hydrochloride. Background technique [0002] Tirofiban hydrochloride CAS registration number: 150915-40-5, the compound structural formula is as follows: [0003] [0004] Tirofiban hydrochloride is a non-peptide platelet glycoprotein IIb / IIIa receptor antagonist, which has anti-platelet aggregation effect and is suitable for patients with unstable angina or non-Q wave myocardial infarction to prevent cardiac ischemia It is also applicable to patients with coronary ischemic syndrome undergoing coronary angioplasty or intracoronary atherectomy to prevent cardiac ischemic complications related to sudden occlusion of treated coronary arteries. [0005] The preparation technology of tirofiban hydrochloride is mainly based on the document Tetrahedron, 1993,49,5767-5776: with N-butanesulfonyl-L-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/22
CPCC07D211/22
Inventor 陈彤李浩源吴鹏程谢卫锋
Owner 无锡富泽药业有限公司
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