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Method for preparing rifampicin crystal form II

A technology of rifampicin and vested rifampicin, applied in the field of rifampicin crystal forms, can solve the problems such as unfavorable recovery and reuse of crystallization solvent, low yield, increased production cost and the like

Inactive Publication Date: 2018-06-01
TIANSHENG PHARMA GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The longest crystallization time of this method is 24 hours, the crystallization time is longer, the product crystallization yield is 70-78%, the yield is not high, and the production cost is increased at the same time, and the mixed solvent crystallization is not conducive to the recovery and reuse of the crystallization solvent

Method used

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  • Method for preparing rifampicin crystal form II
  • Method for preparing rifampicin crystal form II
  • Method for preparing rifampicin crystal form II

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]Under the temperature condition of 25°C and stirring speed of 60r / min, within 30min, add 200g of crude rifampicin raw material into 2000mL acetone in three batches, and stir at this temperature for 3h. Dry under reduced pressure (vacuum degree: 0.08MPa) for 3 hours to obtain 186.3 g of rifampicin crystal form product with a yield of 93.15%. The purity is 98.2%.

[0025] Test instrument conditions: Bruker D2 PHASER powder diffractometer is used for normal temperature test, the test conditions are: Cu Ka It is the light source, the voltage is 30kV, the current is 10mA, the test step is 0.014°, the scanning speed is 0.1s / step, and the scanning range is 5-40° (2θ). After testing, the X-ray powder diffraction pattern of the rifampicin crystal product prepared in Example 1 of the present invention is as follows: figure 1 As shown, the diffraction angle 2θ is at 5.0°, 7.1°, 7.9°, 9.3°, 9.9°, 11.2°, 12.7°, 12.9°, 13.5°, 14.1°, 15.7°, 17.0°, 18.0°, 19.0°, 20.0 °, 21.1°, 21.4°...

Embodiment 2

[0028] At a temperature of 35°C and a stirring speed of 45r / min, add 250g of crude rifampicin into 1250mL of acetone in two batches within 30min, and stir at this temperature for 2h. Dry under reduced pressure (vacuum degree: 0.06MPa) for 1 hour to obtain 225.5 g of rifampicin crystal product with a yield of 90.2%. The product purity is 98.0%.

[0029] The rifampicin crystal prepared in Example 2 was tested with reference to the test method of Example 1, and the results showed that the diffraction angle 2θ was 5.0 ± 0.1 °, 7.0 ± 0.1 °, 7.9 ± 0.1 °, 9.3 ± 0.1 °, 9.9 ± 0.1 °, 11.1±0.1°, 12.6±0.1°, 12.8±0.1°, 13.4±0.1°, 14.1±1°, 15.7±0.1°, 17.0±0.1°, 18.0±0.1°, 18.9±0.1°, 19.9±0.1°, There are characteristic diffraction peaks at 21.0±0.1°, 21.4±0.1°, 22.2±0.1°, 23.1±0.1°, 24.0±0.1°, 25.7±0.1°, 26.2±0.1°, 27.6±0.1°, 30.1±0.1°. The infrared wavelength of the product is 773, 810, 840, 895, 974, 1000, 1023, 1047, 1096, 1118, 1158, 1255, 1375, 1427, 1559, 1643, 1714, 1731, 2883, 2936...

Embodiment 3

[0031] At a temperature of 32°C and a stirring speed of 65r / min, add 190g of crude rifampicin into 2850mL of acetone in two batches within 30min, and stir at this temperature for 1.5h. Dry under reduced pressure (vacuum degree is 0.1MPa) for 2 hours to obtain 173.66 g of rifampicin crystal product with a yield of 91.4%. The product purity is 98.3%.

[0032] The rifampin crystal prepared in Example 3 was tested with reference to the test method of Example 1, and the results showed that the diffraction angle 2θ was 5.0 ± 0.1 °, 7.0 ± 0.1 °, 7.9 ± 0.1 °, 9.3 ± 0.1 °, 9.9 ± 0.1 °, 11.1±0.1°, 12.6±0.1°, 12.8±0.1°, 13.4±0.1°, 14.1±1°, 15.7±0.1°, 17.0±0.1°, 18.0±0.1°, 18.9±0.1°, 19.9±0.1°, There are characteristic diffraction peaks at 21.0±0.1°, 21.4±0.1°, 22.2±0.1°, 23.1±0.1°, 24.0±0.1°, 25.7±0.1°, 26.2±0.1°, 27.6±0.1°, 30.1±0.1°. The infrared wavelength of the product is 774, 807, 841, 896, 973, 998, 1021, 1051, 1096, 1122, 1156, 1254, 1376, 1428, 1560, 1643, 1716, 1730, 2883, 29...

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Abstract

The invention provides a method for preparing rifampicin crystal form II. The method comprises the steps: under the condition of 25 DEG C to 35 DEG C, dissolving a rifampicin crude product into acetone at a stirring speed as 45r / min to 65r / min to be prepared into a solution with a concentration as 0.04g / mL to 0.2g / mL; then under the condition of 25 DEG C to 35 DEG C, continuing stirring for 0.5 to3h at 45r / min to 65r / min; filtering, washing and drying under reduced pressure obtained rifampicin crystal slurry to obtain the rifampicin crystal form II product. A product yield is larger than 90%,and a purity is 98% or more. The method disclosed by the invention has the advantages of stable technology, simpleness in operation, moderate condition, high product yield and purity, good fluidity,low cost, suitability for industrial production and good application prospect.

Description

technical field [0001] The present invention relates to rifampicin crystal form, in particular to a method for preparing rifampicin crystal form II. Background technique [0002] Rifampicin, English name: Rifampicin, chemical name: 3-[[(4-methyl-1-piperazinyl)imino]methyl]-rifamycin, molecular formula is C 43 h 58 N 4 o 12 , Molecular weight: 822.95, rifampicin is bright red or dark red crystalline powder, odorless. Dissolved in methanol, almost insoluble in water. The structural formula of rifampicin is shown below. [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, especially against Mycobacterium tuberculosis and some non-tuberculous mycobacteria. Rifampicin not only has good antibacterial effect on aerobic Gram-positive bacteria and negative bacteria including Streptococcus pneumoniae, Staphylococcus enzyme-producing strains, N...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/08
CPCC07D498/08C07B2200/13
Inventor 刘群谈宗华郭彬邬宁远吴志峰吴统选
Owner TIANSHENG PHARMA GROUP
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