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Novel crystal form of valnemulin hydrogen tartrate and preparation method thereof

A technology of nimulin crystal form and tartaric acid, which is applied in the field of new warnemulin tartrate crystal form and its preparation, can solve the problems of unfavorable premixing agent use, XRD peak strength and low crystallinity, and achieve good fluidity and crystal The effect of uniform particle size distribution and high crystallinity

Active Publication Date: 2014-04-30
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although such commercially available products are crystals, their purity is only about 95%, their crystallinity is not high, their XRD peak intensity is relatively weak, and their solubility in water is only 5g / 100mL at room temperature, which is not conducive to making premixes. Therefore, it is particularly important to develop a new crystal form of warnimulin tartrate with high crystallinity and high water solubility.

Method used

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  • Novel crystal form of valnemulin hydrogen tartrate and preparation method thereof
  • Novel crystal form of valnemulin hydrogen tartrate and preparation method thereof
  • Novel crystal form of valnemulin hydrogen tartrate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 5 g of warnemulin tartrate with a purity of 98% to a crystallizer filled with 10 mL of N,N-dimethylformamide and 90 mL of methyl acetate mixed solvent, stir at 50°C until it dissolves completely, and then drop Add 100mL of methyl acetate eluent to carry out elution and crystallization, and the dropping rate is 0.5mL / min. Then conduct cooling crystallization at a cooling rate of 10°C / h, lower the temperature to 10°C, stir and grow the crystal for 1 hour, carry out suction filtration and washing, and dry the filter cake at 20°C and a vacuum degree of 0.08MPa for 24 hours to obtain the new crystal form of vornimulin tartrate . The process mass yield is 91.5%, the crystal particle size is 15 μm, and the purity is 98.5%. The XRD pattern of the obtained product has characteristic peaks at diffraction angles 2θ=2.48, 4.85, 7.41, 7.53, 10.01, 11.21, 11.70, 13.82 and 17.12 degrees, and the DSC pattern There is a characteristic peak at 101.2°C. The product has good water so...

Embodiment 2

[0032] Add 6 g of warnemulin tartrate with a purity of 96% to a crystallizer filled with a mixed solvent of 15 mL N,N-dimethylformamide and 85 mL ethyl acetate, stir at a constant temperature at 40°C until it dissolves completely, and then drop Add 150 mL of ethyl acetate eluting agent to carry out elution and crystallization, and the dropping rate is 1.5 mL / min. Then carry out cooling and crystallization at a cooling rate of 3°C / h, lower the temperature to 15°C, stir and grow the crystal for 2h, carry out suction filtration and washing, and dry the filter cake at 30°C and vacuum degree of 0.04MPa for 12h to obtain the new crystal form product of vornimulin tartrate . The process mass yield is 92.0%, the crystal particle size is 18 μm, and the purity is 99.0%. The XRD pattern of the obtained product has characteristic peaks at diffraction angles 2θ=2.45, 4.83, 7.41, 7.43, 10.01, 11.28, 11.65, 13.85 and 17.18 degrees, and the DSC pattern There is a characteristic peak at 102.3...

Embodiment 3

[0034]Add 7g of warnemulin tartrate with a purity of 97% to a crystallizer containing 15mL of N,N-dimethylformamide and 85mL of butyl acetate mixed solvent, stir at a constant temperature at 50°C until it dissolves completely, then drop Add 200mL of butyl acetate eluting agent to carry out elution and crystallization, and the dropping rate is 4mL / min. Then carry out cooling and crystallization at a cooling rate of 12°C / h, lower the temperature to 5°C, stir and grow the crystal for 1 hour, carry out suction filtration and washing, and dry the filter cake at 20°C and a vacuum degree of 0.06MPa for 18 hours to obtain a new crystal form product of vornimulin tartrate . The process quality yield is 93.5%, the crystal particle size is 20 μm, and the purity is 98.7%. The XRD pattern of the obtained product has characteristic peaks at diffraction angles 2θ=2.44, 4.87, 7.48, 7.56, 10.05, 11.27, 11.72, 13.84 and 17.13 degrees, and the DSC pattern There is a characteristic peak at 100.7...

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Abstract

The invention relates to a novel crystal form of valnemulin hydrogen tartrate and a preparation method thereof. The method comprises the steps of dissolving valnemulin hydrogen tartrate with the purity being over 95% into a mixed solvent of an ester solvent and N,N-dimethylformamide, adding an elution agent after complete dissolution so as to carry out elution crystallization, then, cooling a solution to the temperature of 5-15 DEG C, and washing, filtrating and drying crystal slurry, thereby obtaining a valnemulin hydrogen tartrate product. An X-ray powder diffraction atlas of the crystal has characteristic peaks when a diffraction angle 2[theta] is equal to 2.5, 4.8, 7.4, 7.5, 10.1, 11.2, 11.7, 13.8 or 17.1 degrees. According to the novel crystal form, during crystallization, the yield reaches over 90%, the product purity reaches over 98%, the product is high in crystallinity, good in stability, difficult in moisture absorption and high in solubility, the water solubility at normal temperature reaches 6.5g / 100mL and is increased by about 30% compared with that of the currently marketed products, and the water stability is good, so that the product can be conveniently prepared into a premix.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a new crystal form of warnimulin tartrate and a preparation method thereof. Background technique [0002] Valnemulin tartrate, also known as Valnemulin hydrogen tartrate, the English name is Valnemulin Hydrogen Tartrate, the molecular formula is C 35 h 58 N 2 o 11 S or C 31 h 52 N 2 o 5 S·C 4 h 6 o 6 , the molecular weight is 714.9, it is a white powder, slightly irritating, and its structural formula is as follows: [0003] [0004] Molecular formula C of Valnemulin 31 h 52 N 2 o 5 S, whose structural formula is as follows, is a new generation of pleuromutilin semi-synthetic antibiotics, which belongs to diterpenes, and is a special antibiotic for animals. positive bacterial infection. It is mainly concentrated in the lungs and is an ideal drug for treating various mycoplasma-induced lung diseases. Vernimulin binds to ...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/28C07C59/255C07C51/41
Inventor 郝红勋欧阳金波王静康侯宝红谢闯鲍颖龚俊波尹秋响陈巍张美景
Owner TIANJIN UNIV
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