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Crystal form of Pravastatin Na, and preparation method and application thereof

A technology of pravastatin sodium and crystal, which is applied in the crystal form of pravastatin sodium and its preparation field, can solve the problems of harsh raw material requirements, poor repeatability, and small crystal particle size, and achieve large crystal particle size and simple operating conditions Easy to control, high crystallinity effect

Inactive Publication Date: 2012-07-11
TIANJIN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that the raw material requirements are harsh, and pravastatin sodium in a specific crystal form is required as a raw material
And the drying process needs to be graded and dried, which is more cumbersome
[0012] A.P.Marti'n-Isla'n et al. reported the M crystal form of pravastatin sodium and its preparation method. The product was obtained by evaporating the solvent. It was verified by experiments that the repeatability was not strong
[0013] In addition to the above operating restrictions, it has been verified by experiments that the products obtained by various methods in the literature generally have shortcomings such as small crystal size, viscous crystal slurry, and difficult filtration.

Method used

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  • Crystal form of Pravastatin Na, and preparation method and application thereof
  • Crystal form of Pravastatin Na, and preparation method and application thereof
  • Crystal form of Pravastatin Na, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 3.50 g of pravastatin sodium to 14 g of N,N-dimethylformamide solvent, heat up to 30° C. to dissolve it, and obtain a transparent light yellow solution. 42 g of ethyl acetate was added under stirring to crystallize. Cool to 0°C at 6min / °C, then continue stirring for 1h. The obtained light yellow suspension was vacuum-filtered, and the filtration speed was fast, and the filter cake was vacuum-dried at 40° C. to obtain 3.25 g of light yellow needle-shaped U-shaped crystals of pravastatin sodium. The product has high crystallinity, large crystal size and smooth surface.

[0040] The XRD pattern of the product is as follows figure 1 As shown, at diffraction angles 2θ°=3.3, 5.6, 6.0, 6.4, 6.8, 8.5, 9.1, 10.1, 11.6, 12.0, 13.7, 14.3, 14.9, 15.5, 17.2, 17.8, 19.0, 20.2, 20.7, 21.3, and There is a characteristic peak at 22.2. Infrared absorption spectrum such as figure 2 Shown at 637, 687, 741, 781, 824, 843, 854, 913, 938, 965, 1015, 1039, 1091, 1109, 1158, 1185, 126...

Embodiment 2

[0042] Put 2.50g of pravastatin sodium into 12g of acetamide solvent, raise the temperature to 40°C, and stir to make it completely dissolved. 100 g of ethyl acetate was added under continuous stirring, and then the resulting suspension was stirred for 1 h. The suspension was filtered, and the filter cake was vacuum-dried at 50° C. to obtain 2.20 g of pale yellow needle-shaped U-shaped crystals of pravastatin sodium.

Embodiment 3

[0044] Put 5.00 g of pravastatin sodium into 15 g of N,N-dimethylformamide solvent, raise the temperature to 90° C., and stir to make it completely dissolved. 120 g of ethyl acetate was added under continuous stirring. The temperature was lowered to 30° C. at 10 min / ° C., and then the resulting suspension was stirred for 0.5 h. The resulting suspension was filtered and dried under vacuum at 70° C. to obtain 4.71 g of pale yellow U-shaped crystals of pravastatin sodium.

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Abstract

The present invention relates to a crystal form of Pravastatin Na, and a preparation method and application thereof. The crystal form is named as a U crystal form. In an X-ray powder diffraction pattern, diffraction angle of 20 degrees, infrared spectrum and endothermic peak in the curve characteristic of a differential scanning calorimeter are defined. The Pravastatin Na in any forms is dissolved in an acid amide solvent to form a solution, the temperature is preferably 30 to 90 DEG C, and the mass ratio of the acid amide solvent to the Pravastatin Na is preferably 3 to 7:1; a dissolving agent is added in the Pravastatin Na solution, the mass of the dissolving agent is 3 to 15 times of that of the solvent, and then a suspension is formed; the suspension is separated and dried, and the U crystal form of the Pravastatin Na is obtained. Through the XRD pattern and the photographs of a scanning electron microscope, it is confirmed that the product has the advantages of high crystallinity, large crystal size, smooth crystal surface and high filtering speed, and the filtering time of crystal mush with the same density and same volume can be saved by more than one half. The U-form Pravastatin Na crystal as a medicine composite has the purpose of treating atherosclerosis or hypercholesterolemia.

Description

technical field [0001] The invention belongs to the technical field of medicine crystallization. In particular, it relates to a crystal form of pravastatin sodium and a preparation method and application thereof. Background technique [0002] The chemical name of pravastatin sodium is 1,2,6,7,8,8a-hexahydro-β,δ,6-trihydroxy-2-methyl, 8-(2-methyl-1-oxobutoxy )-1-Neptanoic acid monosodium salt, the English name is 1-naphthaleneheptanoid acid, 1, 2, 6, 7, 8, 8a-hexahydro-β, δ, 6-trihydroxy-2-methyl-8-(2- methyl-1-oxobutoxy)-, mono sodium salt, the structural formula is as follows, [0003] [0004] Pravastatin is a competitive inhibitor of 3-hydroxy-3-methylglutaryl coenzyme A reductase (HMG-CoA reductase), which can inhibit cholesterol synthesis and has obvious lipid-lowering effect. It is clinically used in diet Limit primary hypercholesterolemia that is still uncontrolled, and at the same time inhibit inflammation, improve vascular endothelial function, stabilize plaqu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/22C07C67/48A61K31/22A61P9/10A61P3/06
Inventor 尹秋响贾海燕高霄梁张美景龚俊波侯宝红
Owner TIANJIN UNIV
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