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Preparation method of crystal form II rifampin

A technology of rifampicin and crystal form, which is applied in the crystallization field of chemical engineering industry, can solve the problems of unspecified crystallization method and operating conditions, small particle size of crystal products, generation of waste acid solution, etc., and achieve good fluidity and crystal form Regular, easy-to-filter effects

Active Publication Date: 2017-09-15
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method does not describe the crystallization method and operating conditions in detail, and its disadvantage is that the crystallization process is under acidic conditions, which will produce a waste acid solution, and the crystal product has a small particle size
[0007] The production process for preparing II crystal form rifampicin in the prior art, they all use high temperature to dissolve the raw material in acetone, and then obtain the II crystal form rifampicin product through evaporation / cooling and cooling crystallization, and the product has a small bulk density, 0.5g / mL, the average particle size is small, about 60μm, and the distribution is uneven, such as figure 1 As shown, problems such as high energy consumption and long time consumption

Method used

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  • Preparation method of crystal form II rifampin
  • Preparation method of crystal form II rifampin
  • Preparation method of crystal form II rifampin

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 100mL of ethanol, add 4g of Rifampicin I crystal form under stirring to form a suspension, stir at 40°C for 2h to carry out solvent-mediated crystallization, filter the suspension, and dry the obtained product at 20°C under a vacuum of 0.1MPa After 10h, 3.65g of Rifampicin in Form II was obtained. The yield after drying the raw material was 91.25%. The product had a high degree of crystallinity, a purity of 99.3%, a main particle size of 138μm, a bulk density of 0.68g / mL, uniform particle size, good fluidity, and was stopped Angle 40°.

[0028] The powder X-ray diffraction pattern of the product is as figure 2As shown, there are characteristic peaks at diffraction angles 2θ=4.9, 7.0, 7.8, 8.8, 9.9, 11.1, 12.6, 13.4, 14.1, 15.7, 16.7, 17.9, 19.9, 21.5, 23.1, 25.1, 25.8, 26.9, 30.0 degrees ; Its TGA analysis such as image 3 As shown, there is no weight loss, and there is a characteristic peak at 194°C.

Embodiment 2

[0030] Take 100 mL of methanol, add 15 g of Rifampicin Form I under stirring to form a suspension, stir at 30°C for 4 hours for solvent-mediated crystallization, filter the suspension, and dry the obtained product at 30°C under a vacuum of 0.05 MPa 8h, 13.6g of rifampicin in Form II was obtained, and the yield after drying the raw material was 90.67%. The product had a high degree of crystallinity, a purity of 99.1%, a main particle size of 137μm, a bulk density of 0.68g / mL, uniform particle size, good fluidity, and stopped Angle 40.3°.

[0031] The powder X-ray diffraction pattern of the product is at diffraction angles 2θ=4.9, 6.9, 7.8, 8.9, 9.9, 11.1, 12.4, 13.5, 14.2, 15.7,, 16.7, 18.0, 19.9, 21.5, 22.8, 25.1, 25.8, 26.9, There is a characteristic peak at 30.1°C; its TGA analysis shows that there is no weight loss, and there is a characteristic peak at 195°C.

Embodiment 3

[0033] Take 100mL of acetonitrile, add 25g of rifampicin of crystal form I under stirring to form a suspension, stir at 45°C for 1 hour for solvent-mediated crystallization, filter the suspension, and dry the obtained product at 50°C under a vacuum of 0.09MPa In 1h, 22.7g of Rifampicin in Form II was obtained. The yield after drying the raw material was 90.8%. The product had a high degree of crystallinity, a purity of 99.0%, a main particle size of 110μm, a bulk density of 0.64g / mL, uniform particle size, good fluidity, and was stopped Angle 40.7°.

[0034] The powder X-ray diffraction pattern of the product is at diffraction angle 2θ=4.9, 6.9, 7.9, 8.9, 9.9, 11.1, 12.5, 13.3, 14.3, 15.7, 16.7, 18.1, 19.9, 21.6, 22.9, 25.1, 25.7, 26.8, 30.0 There are characteristic peaks at the temperature; its TGA analysis shows that there is no weight loss, and it melts (decomposes) at 194°C.

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Abstract

The invention relates to a preparation method of crystal form II rifampin. The method comprises the following steps: adding crude crystal form I rifampin into an organic solvent at 25-45 DEG C while stirring to form a suspension, and stirring the suspension for 1-6 h to carry out solvent mediated crystal transformation; and separating and drying the obtained suspension to obtain the crystal form II rifampin product. The suspension can be cooled to 5-15 DEG C before being separated in order to further increase the yield. The average granularity of the crystal form II rifampin prepared through the solvent mediated crystal transformation technology reaches about 130 [mu]m, the bulk density is more than 0.65 g / mL, and the product has uniform particle size distribution and a structured crystal form, and is easy to filter. The product has good fluidity, the angle of repose is about 40.4 DEG, the purity is more than 99.0%, and the process yield is more than 90.0%. The method has the advantages of simplicity in operation, short time and low energy consumption.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industry crystallization, and in particular relates to a preparation method of rifampicin II crystal form. Background technique [0002] The chemical name of rifampicin is 3-[[(4-methyl-1-piperazinyl)imino]methyl]-rifamycin. The molecular formula is: C 43 h 58 N 4 o 12 , Molecular weight: 822.95, CAS number: 13292-46-1, appearance is bright red or dark red crystalline powder. The structural formula is as follows: [0003] [0004] Rifampicin is a semi-synthetic broad-spectrum antibacterial drug of the rifamycin class, which has antibacterial activity against a variety of pathogenic microorganisms. The mechanism of action of rifampicin is to inhibit the synthesis of bacterial RNA by firmly binding to the β subunit of RNA polymerase, and finally terminate the synthesis of DNA and protein in bacteria. In 1966, Maggi and others from the Italian Leptit company successfully develo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/08
CPCC07B2200/13C07D498/08
Inventor 侯宝红郭楠楠郝红勋张美景徐昭谢闯
Owner TIANJIN UNIV
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