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Crystalline warnemulin hydrochloride product and crystallization preparation method thereof

A technology of vorney hydrochloride and forest products, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low acidification process efficiency, low solubility, poor stability, etc. High bulk density and good stability

Active Publication Date: 2017-02-22
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the solubility of inorganic acids in organic solvents is not very large, so the efficiency of the acidification process is low, and the products obtained are also amorphous products
[0009] In order to solve the disadvantages of poor stability and easy moisture absorption of the amorphous vernesalin hydrochloride product, the present invention has successfully developed a crystalline vernesalin hydrochloride product and a new preparation method thereof by ultrasonic cooling and crystallization

Method used

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  • Crystalline warnemulin hydrochloride product and crystallization preparation method thereof
  • Crystalline warnemulin hydrochloride product and crystallization preparation method thereof
  • Crystalline warnemulin hydrochloride product and crystallization preparation method thereof

Examples

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Effect test

Embodiment 1

[0032] 5 g of amorphous warnemulin hydrochloride with a purity of 98% was added to a crystallizer filled with 10 mL of methanol solvent, stirred at a constant temperature of 300 rpm at 40° C. for 1 hour until completely dissolved; then an ultrasonic probe device was inserted for ultrasonication, Ultrasonic power is 1.5kW, and cooling crystallization is carried out at the same time, the cooling rate is 8°C / h, the temperature is lowered to 10°C, and the ultrasonic wave is stopped for 2 hours; continue to stir and grow crystals at 10°C for 1 hour, and then carry out suction filtration and washing; filter cake in Drying for 24 hours under the conditions of 20° C. and a vacuum degree of 0.08 MPa to obtain a crystalline warnemulin hydrochloride product. The mass yield of the crystallization process is 91.5%. The XRD pattern of the resulting product has characteristic peaks at diffraction angles 2θ=8.4,10.5,10.8,11.2,12.2,12.6,15.1,17.8 and 18.5,19.4,20.2,20.8,25.8,27.7,28.4,29.0 deg...

Embodiment 2

[0034]6g of amorphous warnemulin hydrochloride with a purity of 98% was added to a crystallizer filled with 10mL of ethanol solvent, stirred at a constant temperature of 60°C at a stirring rate of 400rpm for 1 hour until completely dissolved; then an ultrasonic probe device was inserted for ultrasonication, Ultrasonic power is 1.6kW, and cooling crystallization is carried out at the same time, the cooling rate is 10°C / h, the temperature is lowered to 5°C, and the ultrasonic wave is stopped for 2 hours; continue to stir and grow crystals at 5°C for 2 hours, and then carry out suction filtration and washing; filter cake in Dry at 20°C and vacuum degree of 0.06MPa for 24 hours to obtain crystalline warnemulin hydrochloride product. The mass yield of the crystallization process is 92.0%. The XRD pattern of the resulting product has characteristic peaks at diffraction angles 2θ=8.5,10.5,10.9,11.3,12.1,12.7,15.0,17.8 and 18.5,19.4,20.3,20.8,25.8,27.8,28.4,29.0 degrees, and the DSC p...

Embodiment 3

[0036] Add 7 g of amorphous warnemulin hydrochloride with a purity of 98% into a crystallizer filled with 10 mL of isopropanol solvent, and stir at a constant temperature of 50° C. at a stirring rate of 500 rpm for 1 hour until completely dissolved; then insert an ultrasonic probe device for Ultrasound, the ultrasonic power is 1.7kW, cooling and crystallization is carried out at the same time, the cooling rate is 12°C / h, the temperature is lowered to 5°C, and the ultrasonic is stopped for 1 hour; continue to stir and grow the crystal at 5°C for 2 hours, and then carry out suction filtration and washing; The cake was dried for 12 hours at 30° C. under a vacuum of 0.02 MPa to obtain a crystalline warnemulin hydrochloride product. The mass yield of the crystallization process is 93.5%. The XRD pattern of the resulting product has characteristic peaks at diffraction angles 2θ=8.5,10.6,10.9,11.3,12.2,12.6,15.1,17.7 and 18.5,19.3,20.2,20.9,25.7,27.8,28.4,29.1 degrees, and the DSC pa...

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Abstract

The invention relates to a crystalline valnemulin hydrochloride product and a crystallization preparation method thereof. The crystalline valnemulin hydrochloride product is defined by characteristic peaks of an X-ray powder diffraction spectrum in 2theta and DSC. The crystallization preparation method comprises the following steps: under the stirring action, at the temperature of 40-60 DEG C, dissolving an amorphous valnemulin hydrochloride raw material in some organic solvent, and stirring for 1 hour to be completely dissolved, wherein the final solution concentration is 0.5-1 g / mL; at the temperature of 40-60 DEG C, stirring and adding an ultrasonic unit into the solution to be subjected to ultrasonic treatment for 1-2 hours; then reducing the solution temperature to the final temperature of 5-15 DEG C at some cooling rate; continuously stirring at the final temperature, growing the grain for 1-2 hours, and washing, filtering and drying crystal mush to obtain the crystalline valnemulin hydrochloride product. The crystalline valnemulin hydrochloride product is relatively white in color, uniform in granularity, good in flowability and stability, low in hygroscopicity, and high in bulk density, and the once through yield during the crystallization process is higher than 90%.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a crystalline warnimulin hydrochloride product and a crystallization preparation method thereof. Background technique [0002] Valnemulin Hydrochloride, the English name is Valnemulin Hydrochloride, the molecular formula is C 31 h 52 N 2 o 5 S·HCl, with a molecular weight of 601.29, is a white powder and is irritating. Its structural formula is as follows: [0003] [0004] Wernimulin hydrochloride is a new generation of pleuromutilin semi-synthetic antibiotics, which belongs to diterpenes and is a special antibiotic for animals. bacterial infection. It is mainly concentrated in the lungs and is an ideal drug for treating various mycoplasma-induced lung diseases. Wernemulin interacts with the 50S subunit on the ribosome of pathogenic microorganisms, thereby inhibiting the synthesis of pathogenic microorganism proteins, leading to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/52C07C319/28
Inventor 郝红勋李旭东欧阳金波王静康刘爱玲侯宝红王永莉尹秋响鲍颖龚俊波谢闯
Owner TIANJIN UNIV
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