A novel industrial crystallization method of cefathiamidine and its preparation

A cefathiamidine and industrial crystallization technology, applied in the field of medicine, can solve the problems of unstable quality, many impurities and few impurities, and achieve the effects of high separation efficiency, high crystallization efficiency and short crystallization time

Active Publication Date: 2016-02-03
HAINAN LINGKANG PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to solve the problems of poor purity, many impurities and unstable quality in the existing cefathiamidine, aim at simplifying the process and improving efficiency, and provide a kind of cefathiamidine crystallization technology and equipment available for industrialization. The cefathiamidine product refined with equipment has high purity, less impurities and good stability

Method used

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  • A novel industrial crystallization method of cefathiamidine and its preparation
  • A novel industrial crystallization method of cefathiamidine and its preparation
  • A novel industrial crystallization method of cefathiamidine and its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Weigh 6.79 kg of cefathiamidine crude product with a purity of 84.6% and place it in the extraction tank, add 60 kg of methanol-acetone mixed solvent with a volume ratio of 4:1, control the temperature at 50° C., and stir to dissolve it;

[0045] (2) Pump in the alkane fluid to 50Mpa with a high-pressure liquid pump, stir, and keep the pressure and temperature for 30 minutes, and turn off the high-pressure pump;

[0046] (3) Place crystal seeds in the crystallization pool, raise the height of the extraction pool to 30cm, open the quick interface of the two pools, let the liquid in the extraction pool enter the crystallization pool, and close the quick interface;

[0047] (4) Adjust the pressure in the crystallization tank to be 1Mpa, the temperature is 20°C, and keep this temperature and pressure for 40 minutes;

[0048] (5) After the system is cooled down and the pressure is released, dry under reduced pressure to obtain 5.16 kg of high-purity cefathiamidine crystall...

Embodiment 2

[0051] (1) Weigh 6.44 kg of cefathiamidine crude product with a purity of 84.6% and place it in the extraction tank, add 60 kg of methanol-acetone mixed solvent with a volume ratio of 1:2, control the temperature at 40°C, and stir to dissolve it;

[0052] (2) Pump in the alkane fluid to 30Mpa with a high-pressure liquid pump, stir, and keep the pressure and temperature for 10 minutes, and turn off the high-pressure pump;

[0053] (3) Place crystal seeds in the crystallization pool, raise the height of the extraction pool to 30cm, open the quick interface of the two pools, let the liquid in the extraction pool enter the crystallization pool, and close the quick interface;

[0054] (4) Adjust the pressure in the crystallization tank to 0.1Mpa, the temperature is 10°C, and keep the temperature and pressure for 20 minutes;

[0055] (5) After cooling down the system and releasing the pressure, dry under reduced pressure to obtain 4.87 kg of high-purity cefathiamidine crystalline pr...

Embodiment 3

[0058] (1) Weigh 5.66 kg of cefathiamidine crude product with a purity of 84.6% and place it in the extraction tank, add 60 kg of methanol-acetone mixed solvent with a volume ratio of 1:1, control the temperature at 40° C., and stir to dissolve it;

[0059] (2) Pump in the alkane fluid to 40Mpa with a high-pressure liquid pump, stir, and keep the pressure and temperature for 20 minutes, and turn off the high-pressure pump;

[0060] (3) Place crystal seeds in the crystallization pool, raise the height of the extraction pool to 20cm, open the quick interface of the two pools, make the liquid in the extraction pool enter the crystallization pool, and close the quick interface;

[0061] (4) Regulate the pressure in the crystallization tank to be 0.5Mpa, the temperature is 15°C, and keep this temperature and pressure for 30 minutes;

[0062] (5) After the system was cooled down and the pressure was relieved, it was dried under reduced pressure to obtain 4.13 kg of high-purity cefat...

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Abstract

The invention discloses a novel industrial crystallizing technology for cefathiamidine, Recrystallization of the cefathiamidine is achieved by adopting the mode of combining the supercritical fluid extraction technology and the traditional crystallizing technology. In the whole crystallizing system, the process of extraction, adsorption, crystallization and drying is completed under the joint effect of supercritical fluid, a solvent, an extraction pool and a crystallizing pool under the condition of specific temperature and pressure, and recrystallization of the cefathiamidine is achieved. The method is high in separation efficiency and product purity and few in impurities, and greatly improves the quality of preparation products.

Description

technical field [0001] The present invention relates to a novel crystallization technology of cefathiamidine, which belongs to the technical field of medicine. Background technique [0002] In the current market, cefathiamidine, the chemical name is: (6R,7R)-3[(acetoxy)methyl]-7-[α-(N,N'-diisopropylamidinothio)- Acetylamino]-8-oxo-5-thia-1-azabicyclo[4,2,0]oct-2-ene-2-carboxylate betaine, molecular formula: C 19 h 28 N 4 o 6 S 2 , Physical and chemical properties: white or off-white crystalline powder; almost odorless, hygroscopic; easily soluble in water, slightly soluble in ethanol, insoluble in acetone, chloroform or ether. Structural formula: [0003] [0004] Cefathiamidine is the first generation of β-lactam antibiotics. It has antibacterial activity against Gram-positive bacteria and some negative bacteria, especially against Gram-positive cocci. It has good antibacterial effect on Streptococcus viridans, Hemolytic Streptococcus, Non-hemolytic Streptococcus,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/28C07D501/12
CPCC07B2200/13C07D501/12C07D501/28Y02P20/54
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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