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S-Manidipine hydrochloride crystal form I and preparation method thereof

A technology of manidipine hydrochloride, type I, which is applied in the field of pharmaceutical compositions containing it, can solve the problems of low solubility of S-manidipine and the like, and achieves repeatable and controllable production process, stable production process, and crystallinity. good stability

Active Publication Date: 2016-09-07
YANGTZE RIVER PHARMA GRP BEIJING HAIYAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there are no patents and literature reports on the crystal form of S-manidipine. Because S-manidipine has low solubility in the body, it belongs to low-solubility and hypertonic drugs, and its dissolution behavior has a major impact on the effect of the drug in the body. Therefore, its The stability of the crystal form is critical

Method used

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  • S-Manidipine hydrochloride crystal form I and preparation method thereof
  • S-Manidipine hydrochloride crystal form I and preparation method thereof
  • S-Manidipine hydrochloride crystal form I and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Mix 1 gram of S-manidipine free base (prepared according to Chinese patent application 201510870914.8) and 20 ml of absolute ethanol. Then, under stirring, 5 ml of 30% HCl / ethanol solution was added, and the stirring was continued until the solution was completely dissolved. The resulting clear solution was left to stand at room temperature for 8 hours for crystallization, and then filtered to obtain 0.82 g of S-manidipine hydrochloride. Detected by XRD, the crystallization is at about 5.54 (15.97), 6.23 (14.18), 9.56 (9.26), 11.05 (8.00), 11.92 (7.42), 15.16 (5.84), 15.78 (5.62), 18.51 (4.79), 19.54 ( 4.54),20.78(4.27),21.08(4.22),21.75(4.09),22.20(4.00),23.89(3.73),24.67(3.61),24.94(3.57),26.96(3.31),27.38(3.26),29.51( 3.03), there are characteristic peaks at 30.57 (2.92). Its X-ray diffraction pattern is shown in figure 1 , X-ray diffraction data are shown in Table 1 below. Its DSC spectrum is shown in figure 2 , There is a melting endothermic peak at 233.5°C. ...

Embodiment 2

[0059] Mix 1 g of S-manidipine free base and 10 ml of absolute ethanol. Then, under stirring, 5 ml of 30% HCl / ethanol solution was added, and the stirring was continued until the solution was completely dissolved. The resulting clear solution was left to stand at room temperature for 8 hours for crystallization, and then filtered to obtain 0.84 g of S-manidipine hydrochloride. Its XRD and DSC patterns are researched and compared, and it is confirmed that the product is I crystal form.

Embodiment 3

[0061] Mix 1 g of S-manidipine free base and 100 ml of absolute ethanol. Then, under stirring, 5 ml of 30% HCl / ethanol solution was added, and the stirring was continued until the solution was completely dissolved. The resulting clear solution was allowed to stand at room temperature for crystallization for 8 hours, and then filtered to obtain 0.65 g of S-manidipine hydrochloride. Its XRD and DSC patterns are researched and compared, and it is confirmed that the product is I crystal form.

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Abstract

The invention relates to an S-Manidipine hydrochloride crystal form I and a preparation method thereof. The preparation method includes: dissolving S-Manidipine free alkali into alcohols or alcohol / water, salifying with HCL, and crystallizing to obtain S-Manidipine hydrochloride crystal which is determined as the crystal form I according to X-ray powder diffraction detection. Products of the S-Manidipine hydrochloride crystal form I have excellent temperature and humidity stability, meet quality requirements on residual solvent and moisture and are suitable for preparation process and long-term storage. Pharmaceutical compositions with compounds of the crystal form I serving as active ingredients can be used for treating diseases such as hypertension and the like.

Description

technical field [0001] The present invention relates to I crystal form of S-manidipine hydrochloride and its preparation method, as well as its pharmaceutical composition and its medical use. Background technique [0002] The chemical name of S-manidipine hydrochloride is (4S)-1,4-dihydro-2,6-dimethyl-4-m-nitrophenyl-3,5-pyridinedicarboxylate 2- (4-benzhydryl-1-piperazinyl) ethyl ester hydrochloride, its structure is shown in the following formula (I), [0003] [0004] Manidipine hydrochloride is a lipophilic third-generation calcium channel antagonist, a dihydropyridine antihypertensive drug developed by Japan's Takeda Pharmaceutical Co., Ltd. in 1990. This product has high selectivity to blood vessels, which can relax peripheral blood vessels and reduce blood pressure, but has almost no inhibitory effect on the heart. In addition, it has no obvious effect on the level of norepinephrine, suggesting that this product does not activate the sympathetic nervous system. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/90A61K31/496A61P9/12A61P9/10A61P13/12
CPCC07B2200/13C07D211/90
Inventor 刘玉海王建耀刘伟陈东袁峰泉刘文东
Owner YANGTZE RIVER PHARMA GRP BEIJING HAIYAN PHARMA
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