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Cefradine compound prepared by adopting high-flux medicine crystal form rapid screening technology and preparation thereof

A cefradine and compound technology, which is applied in the field of cefradine compounds and preparations thereof, can solve the problems of poor thermodynamic stability, high impurity content, low crystallization yield and the like

Inactive Publication Date: 2017-02-22
陕西顿斯制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to the relatively backward level of domestic reaction crystallization technology, cephradine crystalline products generally have problems such as low crystallization yield, high impurity content, poor fluidity, and poor thermodynamic stability.

Method used

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  • Cefradine compound prepared by adopting high-flux medicine crystal form rapid screening technology and preparation thereof
  • Cefradine compound prepared by adopting high-flux medicine crystal form rapid screening technology and preparation thereof
  • Cefradine compound prepared by adopting high-flux medicine crystal form rapid screening technology and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: the preparation of cefradine compound

[0029] Add 50ml of water and 15ml of N-methylacetamide into the reactor, and control the temperature of the water bath at 40°C. Add 10.01 g of crude cephradine to the above mixed solution, stir continuously until dissolved, and then adjust the pH value to 3.7 with hydrochloric acid. After the reaction was complete, the liquid was transferred to a crystallizer, cooled to 25° C. in a water bath, and elliptical seed crystals were added to grow the crystals for 3 hours. Slowly add tetrachloromethane to the above solution, and filter; dissolve the above filtrate in 100ml of water, add 0.15g of activated carbon, stir and adsorb for 30min, and filter. Add 200ml of ethanol to the filtrate, stir until it is completely precipitated, and filter; wash the filtrate with 30ml of ethanol×2, and dry it in vacuum at 35°C for 3h to obtain 9.81g of white crystalline powder.

[0030] The X-ray powder diffraction pattern of the product...

Embodiment 2

[0030] The X-ray powder diffraction pattern of the product has characteristic peaks at diffraction angles 2θ of 11.46°, 18.47°, 20.85°, 23.21°, and 29.32°. Solid Fourier Transform Infrared Spectrum at a wavenumber of 3311.2cm -1 , 3021.1cm -1 , 1764.2cm -1 , 1684.5cm -1 , 1604.1cm -1 , 1390.4cm -1 , 1351.2cm -1 , 1276.1cm -1 , 1189.1cm -1 , 1060.4cm -1 ,972.4cm -1 ,827.1cm -1 ,774.1cm -1 , 675.4cm -1 There are characteristic peaks. The DSC decomposition temperature is 250.1°C. It is still a white crystalline powder after being placed at a high temperature of 60°C for 10 days. The thermal stability test result at 60°C shows that the weight change rate is 2.1% in 10 days, and the thermal stability is good. Embodiment 2: the preparation of cefradine compound

[0031]Add 50ml of water and 15ml of N-methylacetamide into the reactor, and control the temperature of the water bath at 40°C. Add 10.02 g of crude cephradine into the above mixture, stir continuously until...

Embodiment 3

[0032] The X-ray powder diffraction pattern of the product has characteristic peaks at diffraction angles 2θ of 11.42°, 18.44°, 20.86°, 23.20°, and 29.35°. Solid Fourier Transform Infrared Spectrum at a wavenumber of 3312.3cm -1 , 3021.7cm -1 , 1764.3cm -1 , 1684.4cm -1 , 1604.2cm -1 , 1390.7cm -1 , 1351.3cm -1 , 1276.3cm -1 , 1189.2cm -1 , 1060.5cm -1 ,972.6cm -1 ,827.3cm -1 ,774.4cm -1 , 675.7cm -1 There are characteristic peaks. The DSC decomposition temperature is 250.2°C. It is still a white crystalline powder after being placed at a high temperature of 60°C for 10 days. The result of thermal stability test at 60°C shows that the weight change rate in 10 days is 2.2%, and the thermal stability is good. Embodiment 3: the preparation of cefradine compound

[0033] Add 50ml of water and 15ml of N-methylacetamide into the reactor, and control the temperature of the water bath at 40°C. Add 10.14 g of crude cephradine to the above mixed solution, stir continuou...

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Abstract

The invention discloses a cefradine compound prepared by adopting a high-flux medicine crystal form rapid screening technology. The 'high-end medicine product refined crystallization technology development and industrialization project' won the second prize of the national scientific and technological process in 2015, and the high-flux medicine crystal form rapid screening technology belongs to one of the high-end medicine product refined crystallization technology. The cefradine compound is measured by adopting X-ray powder diffraction, and main characteristic peaks represented by a diffraction angle 2 theta in an atlas are 11.46+ / -0.2 degrees, 18.47+ / -0.2 degrees, 20.85+ / -0.2 degrees, 23.21+ / -0.2 degrees and 29.32+ / -0.2 degrees. The compound is high in purity, low in impurity content and good in flowability and stability. Meanwhile, the invention discloses a preparation prepared by adopting cefradine, and the preparation is the cefradine for injection. The preparation is simple in preparation process, does not need any excipient, has the better solubility and stability and is smaller in side effect compared with an existing preparation.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a cephradine compound prepared by a high-throughput drug crystal form rapid screening technology and a preparation thereof. Background technique [0002] The R&D and industrialization project of refined crystallization technology for high-end pharmaceutical products of one of the inventors, Tianjin University and Xi'an Lijun Pharmaceutical Co., Ltd., won the second prize of the 2015 National Science and Technology Progress Award. [0003] The high-throughput drug crystal form rapid screening technology is one of the refined crystallization technologies for high-end pharmaceutical products. It aims to break through the blockade of related pharmaceutical product crystal forms and crystallization technology patents at home and abroad, and achieve the level of high-end pharmaceutical product research and development and crystallization technology. Leaped up, reached the i...

Claims

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Application Information

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IPC IPC(8): C07D501/22A61K31/545A61P31/04
CPCC07D501/22A61K9/0019C07B2200/13
Inventor 王坤
Owner 陕西顿斯制药有限公司
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