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Novel crystal form of esmolol hydrochloride and preparation method thereof

A technology of esmolol hydrochloride and crystal form, which is applied in the field of new crystal form and preparation of esmolol hydrochloride, can solve the problems affecting the efficacy of the final product, and achieve stable crystal form properties, strong operability, and dissolution good sex effect

Inactive Publication Date: 2020-10-30
HANGZHOU HUANGSEN BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystalline form is not described, which may affect the potency of the final product

Method used

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  • Novel crystal form of esmolol hydrochloride and preparation method thereof
  • Novel crystal form of esmolol hydrochloride and preparation method thereof
  • Novel crystal form of esmolol hydrochloride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 100ml reaction bottle, add 10g of esmolol hydrochloride, add 10ml of methanol, stir to dissolve, after the solid is completely dissolved, add 50ml of ethyl acetate at 15-25°C, keep at 15-25°C, stir and crystallize for 1-2 hours, Then the temperature was lowered to 0-10°C and stirred for 3-4h, the solid was filtered out, washed with a small amount of ethyl acetate, and vacuum-dried at 40°C for 4-6h to obtain 8.5g of off-white powder with a yield of 85%.

[0029] At ambient temperature and humidity, using Cu-Ka radiation, expressed in 2θ angles X-ray powder diffraction has characteristic peaks at the following positions: 2θ = 5.787°, 11.495°, 12.903°, 13.499°, 15.219°, 16.012°, 17.219 °, 18.238°, 18.924°, 20.535°, 22.159°, 23.014°, 23.745°, 24.316°, 26.311°, 27.675°, 28.887°, 29.93°, 30.973° ​​have characteristic peaks, such as figure 1 shown.

[0030] According to thermogravimetric analysis, the decomposition temperature of the crystal form A of esmolol hydrochlori...

Embodiment 2

[0035] In a 250ml reaction bottle, add 15g of esmolol hydrochloride, add 15ml of methanol, and stir to dissolve. After all the solids are dissolved, keep warm at 15-25°C and add 75ml of isopropyl acetate, keep warm at 15-25°C, stir and crystallize for 1-2 hour, then lower the temperature to 0-10°C and stir for 3-4h, filter out the solid, wash with a small amount of ethyl acetate, and vacuum-dry at 40°C for 4-6h to obtain 13.05g of off-white powder with a yield of 87%.

[0036] At ambient temperature and humidity, using Cu-Ka radiation, expressed in 2θ angles X-ray powder diffraction has characteristic peaks at the following positions: 2θ = 5.791°, 11.505°, 12.993°, 13.511°, 15.234°, 16.117°, 17.385 °, 18.369°, 19.018°, 20.662°, 22.287°, 23.198°, 23.902°, 24.501°, 26.502°, 27.799°, 28.968°, 30.911°, 32.545° have characteristic peaks.

[0037]According to thermogravimetric analysis, the decomposition temperature of the crystal form A of esmolol hydrochloride was 93.32° C., and t...

Embodiment 3

[0040] In a 250ml reaction bottle, add 15g of esmolol hydrochloride, add 30ml of isopropanol, stir to dissolve, after all the solids are dissolved, add 60ml of ethyl acetate at 25°C, keep at 15-25°C, stir and crystallize for 1-2 hours , then cooled to 0-10°C and stirred for 3-4h, filtered the solid, washed with a small amount of ethyl acetate, and dried in vacuum at 40°C for 4-6h to obtain 13.5g of off-white powder with a yield of 90%.

[0041] At ambient temperature and humidity, using Cu-Ka radiation, X-ray powder diffraction has characteristic peaks at the following positions in terms of 2θ angles: 2θ = 5.622°, 11.301°, 12.756°, 13.321°, 15.088°, 15.988°, 17.087 °, 18.099°, 18.796°, 20.388°, 22.004°, 22.886°, 23.596°, 24.156°, 26.159°, 27.495°, 28.706°, 29.759°, 30.795° have characteristic peaks.

[0042] According to thermogravimetric analysis, the decomposition temperature of the esmolol hydrochloride A crystal form A was 93.32 °C, and there was no weight loss before the ...

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Abstract

The invention relates to a novel crystal form of esmolol hydrochloride and a preparation method thereof. The powder X-ray diffraction pattern is has characteristic peaks at the positions of 2theta = 5.787 + / -0.2 degrees, 11.495 + / -0.2 degrees, 12.903 + / -0.2 degrees, 13.499 + / -0.2 degrees, 15.219 + / -0.2 degrees, 16.012 + / -0.2 degrees, 17.219 + / -0.2 degrees, 18.238 + / -0.2 degrees, 18.924 + / -0.2 degrees, 20.535+ / -0.2 degrees, 22.159+ / -0.2 degrees, 23.014 + / -0.2 degrees, 23.745 + / -0.2 degrees, 24.316 + / -0.2 degrees, 26.311 + / -0.2 degrees, 27.675 + / -0.2 degrees, 28.887 + / -0.2 degrees, 29.93 + / -0.2degrees and 30.973 + / -0.2 degrees. The esmolol hydrochloride crystal form prepared by the invention is stable in property, good in solubility and suitable for drug development, and the used preparation method is safe, simple and convenient, and strong in operability.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a new crystal form of esmolol hydrochloride and a preparation method thereof. Background technique [0002] Polymorphism refers to the phenomenon that solid substances form solid states with different physical and chemical properties in two or more different spatial arrangements. In the field of pharmaceutical research, polymorphism includes multi-component crystal forms such as organic solvates and hydrates. Drug polymorphism widely exists in the drug development process and is an inherent characteristic of small organic molecules. Polymorphism is not only controlled by internal factors such as the spatial structure and functional group properties of the molecule itself, intramolecular and intermolecular interactions, but also by drug synthesis process design, crystallization and purification conditions, preparation excipients selection, preparation process, etc. Routes and g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/32C07C213/10
CPCC07B2200/00C07C213/10C07C217/32
Inventor 姚红罗瑾吴晓峰李珲王佳谭艳红万兴隆
Owner HANGZHOU HUANGSEN BIOLOGICAL TECH CO LTD
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