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A kind of warnemulin oxalate crystal and preparation method thereof

A technology of vonimulin and oxalic acid, applied in the field of oxalic acid vonimulin crystals and preparation thereof, can solve the problems of serious hygroscopicity, unstable melting point, small particle size, etc., and achieves good crystal shape, not easy to scatter, and good stability. Effect

Active Publication Date: 2016-01-20
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The warnemulin hydrochloride products obtained by these methods are all amorphous products, and the particle size of the amorphous product is small, and has problems such as serious hygroscopicity, unstable melting point, and easy scattering

Method used

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  • A kind of warnemulin oxalate crystal and preparation method thereof
  • A kind of warnemulin oxalate crystal and preparation method thereof
  • A kind of warnemulin oxalate crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Dissolve 1g of warnemulin in 10mL of ethyl formate, add 0.16g of oxalic acid according to the molar ratio of oxalic acid to warnemulin at 1:1, under stirring, raise the temperature to 60°C to react until clear, then cool down, the cooling rate at 15°C / h, lower the temperature to 10°C, filter, wash with ethyl formate reagent, and dry the filter cake to obtain the warnemulin oxalate crystal product. The process mass yield is 91.5%, the main crystal particle size is 16 μm, and the product purity is 98.5%.

[0033] The XRD figure of gained product has characteristic peak at diffraction angle 2θ=6.21,8.03,10.52,11.34,12.65,13.27,14.70,15.03,17.12,18.14,19.86 and 21.27 degree, and DSC figure has characteristic peak at 122.2 DEG C, pulling Mantu has obvious Raman peaks at 405, 452, 505, 752, 803, 950, 1100, 1210, 1480, 1520, 1630, and 1778. The prepared warnemulin oxalate crystals are not easy to scatter, and have good stability to light, heat and humidity. When the relative...

Embodiment 2

[0035] Dissolve 1g of warnemulin in 10mL of ethyl acetate, add 0.08g of oxalic acid according to the molar ratio of oxalic acid and warnemulin at 1:2, and stir to raise the temperature to 50°C until the reaction is clear, then cool down, the cooling rate 10°C / h, lower the temperature to 15°C, then filter, wash with butyl acetate reagent, dry the filter cake at 40°C, vacuum degree 0.07MPa for 24h, and obtain the warnemulin oxalate crystal product. The process mass yield is 92.3%, the main crystal particle size is 17 μm, and the product purity is 97.5%.

[0036] The XRD figure of gained product has characteristic peak at diffraction angle 2θ=6.12,8.11,10.45,11.38,12.52,13.24,14.73,15.09,17.20,18.17,19.78 and 21.23 degrees, and DSC figure has characteristic peak at 123.4 DEG C, pulling Mantu has obvious Raman peaks at 412, 442, 515, 758, 813, 952, 1150, 1260, 1490, 1510, 1640, and 1758. The prepared warnemulin oxalate crystals are not easy to scatter, and have good stability to ...

Embodiment 3

[0038] Dissolve 2g of warnemulin in 10mL of butyl acetate, add 0.21g of oxalic acid at a molar ratio of oxalic acid to warnemulin of 1:1.5, and stir to raise the temperature to 40°C until clear, then cool down at a rate of 5°C / h, lower the temperature to 20°C, then filter, wash with a mixed reagent of butyl acetate and ethyl acetate, and dry the filter cake at 35°C and a vacuum of 0.06MPa for 12h to obtain the crystalline product of warnemulin oxalate. The process mass yield is 92.5%, the main crystal particle size is 18 μm, and the product purity is 96.5%.

[0039] The XRD figure of gained product has characteristic peak at diffraction angle 2θ=6.15,8.15,10.36,11.29,12.56,13.27,14.69,15.11,17.13,18.14,19.88 and 21.19 degrees, and DSC figure has characteristic peak at 123.7 DEG C, pulling Mantu has obvious Raman peaks at 410, 461, 508, 748, 813, 947, 1121, 1215, 1482, 1524, 1632, and 1768. The prepared warnemulin oxalate crystals are not easy to scatter, have good stability t...

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Abstract

The invention relates to a valnemulin oxalate crystal and a crystallization preparation method thereof. According to an X-ray powder diffraction pattern of the crystal, characteristic peaks appear at diffraction angle 2theta of 6.2, 8.0, 10.5, 11.2, 12.5, 13.2, 14.6, 15.0, 17.0, 18.0, 19.7 and 21.1 degrees. According to the invention, valnemulin is dissolved in an ester type solvent, wherein a solution concentration is 0.1-0.4g / mL; oxalic acid is added according to a molar ratio that oxalic acid to valnemulin is 1:1-1:2; under a stirring effect, a reaction is carried out under a temperature of 40-60 DEG C until the solution is clear; the temperature of the solution is reduced to 10-20 DEG C; and filtering, washing, and drying are carried out, such that a valnemulin oxalate crystal product is obtained. The crystallization process has a yield higher than 90%. The valnemulin oxalate product has high crystallinity, high purity, and low fly-off. The valnemulin oxalate product has good stability against light, heating, and moisture.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a warnimulin oxalate crystal and a preparation method thereof. Background technique [0002] Vernimulin is a new generation of pleuromutilin semi-synthetic antibiotics, which belongs to diterpenes and is a special antibiotic for animals. It has the characteristics of strong antibacterial activity, broad antibacterial spectrum, low residue, and short drug duration, especially for mycoplasma and spirochetes. Due to the advantages of low toxicity, few side effects, fast metabolism, less drug accumulation residue in the body, and less drug-resistant strains, it is mainly used to prevent and treat swine dysentery caused by Brachyspira hyodysenteriae infection and Mycoplasma pneumoniae infection porcine enzootic pneumonia. It is the first European-wide approved veterinary drug premix, listed as a prescription drug for veterinary use. Molecula...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/52C07C319/28
Inventor 郝红勋欧阳金波王静康李旭东刘爱玲侯宝红王永莉尹秋响鲍颖程转红
Owner TIANJIN UNIV
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