Crystal form of lercanidipine hydrochloride and preparation method thereof and crystal form-containing medicinal composition

A technology of Leca hydrochloride and dipine crystals, which is applied in the field of new crystal forms and their preparation methods and pharmaceutical compositions containing the crystal forms, can solve the problems of complex preparation methods, and achieve high purity, good stability and simple methods Effect

Active Publication Date: 2011-04-20
SHENZHEN SALUBRIS PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

US4705797 discloses the synthesis method of lercanidipine, and prepares its hemihydrate and hydrochloride by using dilute hydrochloric acid in the presence of NaCl, but the preparation method is more complicated, and produces undesired by-products and subsequent purification of chromatographic columns

Method used

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  • Crystal form of lercanidipine hydrochloride and preparation method thereof and crystal form-containing medicinal composition
  • Crystal form of lercanidipine hydrochloride and preparation method thereof and crystal form-containing medicinal composition
  • Crystal form of lercanidipine hydrochloride and preparation method thereof and crystal form-containing medicinal composition

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The preparation of embodiment 1 lercanidipine hydrochloride raw material

[0039] The raw material of lercanidipine hydrochloride is according to the method of US4705797, with N-methyl-N-(3,3-diphenylpropyl)-1-amino-2-propanol and diketene as raw materials, after esterification and condensation, and The crude lercanidipine in the form of oil was prepared by cyclization of methyl β-aminobutyrate. After purification, the purity analysis by HPLC was 85.0%-99.5%, which was used as a raw material for subsequent preparation.

Embodiment 2

[0040] The preparation of embodiment 2 lercanidipine hydrochloride crystal forms

[0041]10g of lercanidipine hydrochloride with a purity of 99.5% was dissolved in methanol, evaporated to dryness until oily, added acetone: isopropyl acetate = 1:2, 500ml, stirred and dissolved, kept refrigerated at 0-5°C, pumped after 12 hours filtered, and vacuum dried at 70°C for 24 hours to obtain 8.8 g of the new crystalline product with a purity of 99.9%. The X-ray diffraction spectrum of gained new crystal form product, infrared spectrum (IR) collection of illustrative plates and differential scanning calorimetry (DSC) collection of illustrative plates are respectively as follows figure 1 , figure 2 and image 3 shown.

Embodiment 3

[0042] The preparation of embodiment 3 lercanidipine hydrochloride crystal forms

[0043] 10g of lercanidipine hydrochloride oily matter with a purity of 85% was added with acetone: isopropyl acetate=1: 30, 50ml, after stirring to dissolve, the new crystal seed crystal obtained as in Example 2 was added, and after stirring at room temperature for 12 hours Suction filtration and vacuum drying at 70°C for 24 hours gave 8.3 g of the new crystalline product with a purity of 99.5%.

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Abstract

The invention provides a novel crystal form of lercanidipine hydrochloride, which has peaks at 5.38 DEG, 10.74 DEG, 11.54 DEG, 11.88 DEG, 15.14 DEG, 17.26 DEG, 17.92 DEG, 19.82 DEG, 20.22 DEG, 20.70 DEG, 21.44 DEG, 21.98 DEG and 22.56 DEG expressed by a 2theta angle in an X ray diffraction pattern. The novel crystal form has high purity (over 99.5 percent) and high stability, has low rigidity and is easy to crush after being dried, and facilitates preparing and using a medicinal composition. The invention also provides a preparation method for the crystal form and a crystal form-containing medicinal composition. Compared with the prior art, the preparation method has the advantages of simple process, mild preparation conditions and high yield.

Description

technical field [0001] The invention belongs to the field of preparation of pharmaceutical compounds, in particular to a new crystal form of lercanidipine hydrochloride, a preparation method thereof and a pharmaceutical composition containing the crystal form. Background technique [0002] Lercanidipine Hydrochloride, chemical name 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)-3,5-pyridinedicarboxylic acid 2-[(3 , 3-diphenylpropyl) methylamino]-1,1-dimethylethyl methyl ester hydrochloride, its chemical structure is the following formula (I): [0003] [0004] As a dihydropyridine calcium antagonist, lercanidipine hydrochloride can selectively bind to the L-type calcium ion channel receptor on the membrane of vascular smooth muscle cells, inhibiting Ca 2+ Inflow, relaxation of vascular smooth muscle, dilation of blood vessel walls, to achieve antihypertensive effect. Due to its strong fat solubility and short plasma half-life, lercanidipine hydrochloride can play a long-las...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/90A61K31/4422A61P9/12
Inventor 张昌中郑加林
Owner SHENZHEN SALUBRIS PHARMA CO LTD
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