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Novel ivabradine hydrochloride crystal form and its preparation method and use in preparation of pharmaceutical composition

A technology of ivabradine hydrochloride and crystal form, which is applied in the field of medicine to achieve the effect of being conducive to storage, high stability of temperature, humidity and light

Inactive Publication Date: 2012-10-17
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Considering the pharmaceutical value of the compound, it is very important to obtain a high-purity stable crystal form of the compound. The present invention provides a crystal form of ivabradine hydrochloride with high purity and strong stability, which can be easily industrialized and economical. The preparation method of low cost can realize industrialized production very conveniently; The technical problem to be solved in the present invention is to obtain the IHC with excellent purity, complete crystal form, sufficient stability and moderate particle size through the method of solvent recrystallization with low toxicity and low price. Valbradine crystallizes and has sufficient stability for long-term storage without special requirements on temperature, light and oxygen

Method used

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  • Novel ivabradine hydrochloride crystal form and its preparation method and use in preparation of pharmaceutical composition
  • Novel ivabradine hydrochloride crystal form and its preparation method and use in preparation of pharmaceutical composition
  • Novel ivabradine hydrochloride crystal form and its preparation method and use in preparation of pharmaceutical composition

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Embodiment 1

[0032] Heat 100 g of ivabradine hydrochloride with 200 ml of anhydrous ethanol and stir until all is dissolved, stop heating, cool and stir to crystallize, after natural cooling to 21°C, stir and crystallize in an ice water bath at 1°C for 2 hours. After the crystallization is completed, the filter cake is washed with a small amount of absolute ethanol, and the filter cake is dried in a vacuum drying oven at 65°C to a constant weight to obtain a new crystal form of ivabradine hydrochloride with a purity of greater than 99.90%.

Embodiment 2

[0034] Heat 100g ivabradine hydrochloride with 400ml absolute ethanol under reflux and stir until all is dissolved, stop heating, cool and stir to crystallize, after natural cooling to 26°C, stir and crystallize in an ice water bath at 0°C for 3 hours. After the crystallization is completed, the filter cake is eluted with a small amount of absolute ethanol, and the filter cake is dried to a constant weight in a vacuum drying oven at 70°C to obtain a new crystal form of ivabradine hydrochloride with a purity of greater than 99.89%.

Embodiment 3

[0036] Heat 100 g of Ivabradine hydrochloride with 800 ml of ethyl acetate and absolute ethanol (3:1) and stir under reflux until all is dissolved. Stop heating, cool and stir to crystallize. After natural cooling to 25°C, stir under 1°C ice water bath Crystallize for 2h. After the crystallization is completed, the filter cake is washed with a small amount of ethyl acetate, and the filter cake is dried to constant weight in a vacuum drying oven at 71° C. to obtain a new crystal form of ivabradine hydrochloride with a purity of greater than 99.8%.

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Abstract

The invention relates to a novel ivabradine hydrochloride crystal form and its preparation method and use in preparation of a pharmaceutical composition. The preparation method comprises the following steps of carrying out heating reflux stirring of a mixture of ivabradine hydrochloride and anhydrous ethanol, or a mixture of ivabradine hydrochloride, anhydrous ethanol and ethyl acetate until complete dissolution, stopping heating, carrying out natural cooling and stirring for crystallization, and after complete crystallization, carrying out pumping filtration collection of products. The novel ivabradine hydrochloride crystal form can treat or prevent various local myocardial ischemia clinical symptoms such as angina, myocardial infarction and accompanying rhythmic disorder, and also can treat or prevent symptoms related to rhythmic disorder and especially to supraventricular rhythmic disorder.

Description

Technical field [0001] The invention belongs to the technical field of medicine, and specifically relates to a new crystal form of ivabradine hydrochloride, a preparation method and its use in preparing a pharmaceutical composition. Background technique [0002] Ivabradine hydrochloride, chemical name: 3-[3-[[(8S)-3,4-dimethoxy-8-bicyclo[4.2.0]octane-1,3,5-tri En]methyl-methylamino]propyl]-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepine-4-one hydrochloride, the chemical structure is as follows: [0003] [0004] Ivabradine hydrochloride is the first selective and specific If channel blocker developed by the French company Servier. It has a pure heart rate lowering effect and is used for the treatment of normal sinus rhythm and b receptor blockade. Symptomatic treatment of chronic stable angina pectoris that is contraindicated or intolerable. At present, it has been marketed in many European countries and has very valuable pharmacological and therapeutic effects, especially the perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/16A61K31/55A61P9/10
Inventor 赵志全卢传广黄维国
Owner SHANDONG NEWTIME PHARMA
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