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A kind of preparation method of rifampin i crystal form

A technology of rifampicin and crystal form, which is applied in the crystallization field of chemical engineering industry, can solve the problems of poor fluidity of I crystal form rifampicin products, long crystallization operation time, and small product bulk density, and achieve good fluidity and low cost , time-consuming effect

Active Publication Date: 2019-02-22
TIANJIN UNIV
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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 crystallization operation time is long, about 15 hours, and the obtained I crystal form rifampicin product has poor fluidity and is easy to coalesce
[0007] The production process for preparing I crystal form rifampicin in the prior art, they all use high temperature to dissolve the raw material in n-butanol, and then obtain the I crystal form rifampicin product through evaporation / cooling and cooling crystallization, and the product has a small bulk density, About 0.4g / mL, the average particle size is small, about 50μm, the coalescence is serious, if attached figure 1 As shown, problems such as high energy consumption and long time consumption

Method used

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  • A kind of preparation method of rifampin i crystal form
  • A kind of preparation method of rifampin i crystal form
  • A kind of preparation method of rifampin i crystal form

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Take 100mL of n-propanol, add 20g of rifampin in crystal form II under stirring to form a suspension, stir at a constant temperature at 45°C for 4h, perform solvent-mediated crystallization, and filter the suspension. Drying under MPa for 2h, 18.05g of crystal form I rifampicin was obtained. The yield after drying the raw material was 90.25%. Good fluidity, angle of repose 37.2°.

[0031] The I-crystal solvate compound obtained after suspension and crystallization has a TGA figure of weight loss at 40°C, which is a desolvation process, and it decomposes at 251°C, such as figure 2 shown. Obtain I crystal form rifampicin product after drying, and its powder X-ray diffraction pattern is as follows image 3 As shown, there are characteristic peaks at diffraction angles 2θ=7.2, 8.6, 11.7, 13.6, 14.3, 16.2, 18.3, 19.3, 20.4, 21.1, 22.1, 22.7, 24.0, 24.6, 26.0, 27.4, and 29.3 degrees; its TGA analysis like Figure 4 As shown, there is no weight loss, and it decomposes at ...

Embodiment 2

[0033] Take 100 mL of n-butanol, add 35 g of Rifampicin in Form II with stirring to form a suspension, stir at 35°C for 8 hours to perform solvent-mediated crystallization, and then cool the suspension until the temperature is lowered to 5°C. The suspended liquid was filtered, and the obtained product was dried at 40° C. and a vacuum of 0.04 MPa for 5 hours to obtain 32.65 g of crystalline form I rifampicin. The yield after drying the raw material was 93.3%. The product had high crystallinity, a purity of 99.2%, and a primary particle size of 168μm, bulk density 0.52g / mL, uniform particle size, good product fluidity, angle of repose 37.8°.

[0034] The I-crystal solvate compound obtained after suspension and crystallization has a TGA figure of weight loss at 39°C, which is a desolvation process and decomposes at 252°C. After drying, the I crystal form rifampicin product is obtained, and its powder X-ray diffraction pattern is at diffraction angles 2θ=7.2, 8.6, 11.7, 13.5, 14.3...

Embodiment 3

[0036] Take 100mL of n-hexane, add 25g of Rifampin in crystal form II under stirring to form a suspension, stir at a constant temperature at 25°C for 15h, perform solvent-mediated crystallization, and filter the suspension. Dry for 2 hours to obtain 23.1 g of crystalline form I rifampicin. The yield after drying the raw material is 92.4%. The product has a high degree of crystallinity, a purity of 99.1%, a main particle size of 153 μm, a bulk density of 0.57 g / mL, a uniform particle size, and a fluidity of the product. Well, the angle of repose is 36.8°.

[0037] The I-crystal solvate obtained after suspension and crystallization has a weight loss at 42°C in the TGA chart, which is a desolvation process and decomposes at 254°C. After drying, the I crystal form rifampicin product is obtained, and its powder X-ray diffraction pattern is at diffraction angle 2θ=7.2,8.6,11.7,13.6,14.3,16.2,18.2,19.3,20.5,21.2,22.1,22.7,24.0,24.6 , There are characteristic peaks at 26.0, 27.4, and...

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Abstract

The invention relates to a preparation method of crystal form I rifampin. The method comprises the following steps: adding crude crystal form II rifampin into an organic solvent at 25-45 DEG C while stirring to form a suspension, and stirring the suspension for 4-15 h to carry out solvent mediated crystal transformation; and separating and drying the obtained suspension to obtain the crystal form I 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 I rifampin prepared through the solvent mediated crystal transformation technology reaches about 160 [mu]m, the bulk density is more than 0.57 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 37 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 crystallization in the chemical engineering industry, and in particular relates to a preparation method of rifampicin I 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, easily soluble in chloroform, slightly soluble in water. The structural formula is as follows: [0003] [0004] Rifampicin is an important anti-tuberculosis drug, which has antibacterial activity against a variety of pathogenic microorganisms. In 1966, Maggi and others from the Italian Leptit company successfully developed rifampicin by semi-synthetic method for the first time, and it was officially put into production in 1969. In 1972, my country's trial production was successful, and the produc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/08
CPCC07B2200/13C07D498/08
Inventor 侯宝红郭楠楠郝红勋张美景鲍颖徐昭
Owner TIANJIN UNIV
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