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Lercanidipine hydrochloride crystal and preparation method thereof

A technology for lercanidipine hydrochloride and crystal, which is applied in the field of crystal of new form of lercanidipine hydrochloride and its preparation, and can solve the problems of complicated preparation, increasing difficulty and cost of large-scale production, etc.

Active Publication Date: 2012-05-30
CHONGQING SHENGHUAXI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The preparation of the above-mentioned lercanidipine hydrochloride crystals is somewhat complicated. For example, it is necessary to form corresponding solvates with various organic solvents, and then remove the solvents therein under specific conditions (such as vacuum drying or nitrogen-filled drying) to obtain the corresponding forms. crystal products, increasing the difficulty and cost of industrial mass production

Method used

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  • Lercanidipine hydrochloride crystal and preparation method thereof
  • Lercanidipine hydrochloride crystal and preparation method thereof
  • Lercanidipine hydrochloride crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Example 1 Preparation of lercanidipine hydrochloride hydrate

[0028] Take 60 g of the above-mentioned lercanidipine base raw material, dissolve it with 5 times the volume of dichloromethane (or dichloroethane, chloroform), add 5 to 10 times the volume of 10% (w) hydrochloric acid aqueous solution, fully stir and let it stand , separate the water layer, wash the dichloromethane phase with saturated brine, and recover the solvent by distillation or vacuum distillation, add 10 times the volume of water to the residue, stir at room temperature to crystallize, suction filter, wash the solid with water, and dry at 70- Vacuum-dried at 80°C to obtain 50 g of lercanidipine hydrochloride hydrate, with a moisture content of 4.5%, a melting temperature of 110-120°C, and an HPLC purity of ≥95%.

Embodiment 2

[0029] Example 2 Preparation of lercanidipine hydrochloride Form (HX) crystals

[0030] Take 10 g of lercanidipine hydrochloride hydrate obtained in Example 1, add 30 ml of DMF, stir to dissolve completely, then add 200 ml of ethyl acetate dropwise to the solution, then cool the solution to 0-5°C, and continue stirring until the solid is fully separated. , filtered with suction, and the filter cake was vacuum-dried at 70-80°C for 8 hours to obtain 7 g of anhydrous lercanidipine hydrochloride Form (HX) crystals, with HPLC purity ≥ 99%, and a melting temperature of 125°C-142°C. The IR spectrum, X-ray diffraction spectrum and thermal analysis spectrum (DSC, TG diagram) of the product are as follows figure 1 , figure 2 with image 3 shown.

Embodiment 3

[0031] Example 3 Preparation of lercanidipine hydrochloride Form (HX) crystals

[0032] Get the lercanidipine hydrochloride hydrate 10g of embodiment 1, add 40ml DMSO, after stirring to dissolve completely, add dropwise 200ml isopropyl acetate in the solution, then continue to stir at normal temperature until a large amount of solids are precipitated, suction filtration, filter cake Vacuum-dried at 70-80°C for 8 hours to obtain 6 g of anhydrous lercanidipine hydrochloride Form (HX) crystals, with HPLC purity ≥ 99% and melting temperature of 130°C-141°C.

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Abstract

The invention is a lercandipine hydrochloride crystal (form (HX) crystal) and a preparation method. The crystal has no crystalline water and virgule or crystalline solvent, and is a novel high-purity stable crystalline form, which is more suitable for the large-scale industrial production. The invention has advantages of simple and easy operation, and facilities to prepare the drug combination and provides the clinical use. The crystal uses the Cu-K alpha radiation. The X-ray powder diffraction spectra show expressed in the 2-theta angle has the following characteristics: an angle (2 theta), D(A), a peak relative intensity (%): 7.4, 11.9, 47; 9.6, 9.2, 64; 12.6, 7.0, 32; 13.2, 6.7, 36; 15.7, 5.6, 38; 15.9, 5.6, 63; 17.0, 5.2, 64; 21.4, 4.1, 100; 23.6, 3.8, 87; 5, 3.6, 58.

Description

technical field [0001] The invention relates to a crystal of a new form of lercanidipine hydrochloride and a preparation method thereof. The compound is an antihypertensive medicinal compound. Background technique [0002] Lercanidipine Hydrochloride, the chemical name is 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid-3- [β-(N-3,3-diphenylpropyl-N-methylamino)-α,α-dimethyl]ethyl ester-5-methyl ester hydrochloride, chemical structure as shown in formula (I) [0003] [0004] The compound is a lipophilic compound, and as an antihypertensive medicinal compound, it has the characteristics of long action time and good antihypertensive effect, and is clinically administered through an oral route. There have been studies and reports on its crystalline state. [0005] GB 8403866 describes the synthesis method of the above lercanidipine, the final product of which is lercanidipine hydrochloride hemihydrate with a melting point of 119°C-123°C. [0006]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/90
Inventor 何亮贾春荣苏家宏
Owner CHONGQING SHENGHUAXI PHARMA CO LTD
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