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Method utilizing coupling reaction crystallization to prepare cefuroxime sodium

A technology of cefuroxime sodium and coupling reaction, applied in the direction of organic chemistry, can solve the problems of increasing solvent recovery difficulties, insoluble particles, complicated operation, etc., and achieve the effect of reducing adsorption and filtration process, reducing degradation, and uniform particle size

Inactive Publication Date: 2012-08-01
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not control the reaction process, and introduces double eluents in the crystallization process, which increases the difficulty of solvent recovery
Moreover, in the existing cefuroxime sodium preparation process, it is necessary to decolorize by activated carbon adsorption, and insoluble particles may be introduced during the operation, which leads to a decrease in yield and complicated operation.

Method used

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  • Method utilizing coupling reaction crystallization to prepare cefuroxime sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 70ml of acetone and 10ml of pure water into the crystallizer, put in 7g of cefuroxime acid, and stir at 20°C until fully dissolved. 4.4ml of sodium carbonate aqueous solution with a concentration of 0.2g / ml was added dropwise to the cefuroxime acid solution and stirred at constant temperature for 10min to complete the reaction. Add 0.28 g of cefuroxime sodium seed crystal, keep the temperature for 10 minutes, and add 480 ml of acetone dropwise. Then the temperature is lowered to 5°C and kept at a constant temperature for 0.5h. Filtration with suction, washing with acetone, and drying at 20°C and a vacuum degree of 0.08 MPa for 3 hours to obtain cefuroxime sodium product. The color grade of the product is lower than Y1 or YG1, the purity is 99.6%, and the yield is 95.3%.

Embodiment 2

[0021] Add 145ml of acetone and 95ml of ethanol to the crystallizer, add 10g of cefuroxime acid, control the temperature at 25°C and stir until it is completely dissolved. A mixture of 2.2 ml of sodium carbonate aqueous solution with a concentration of 0.3 g / ml and 6.7 ml of sodium isooctanoate aqueous solution was added dropwise to the cefuroxime acid solution and stirred at constant temperature for 15 minutes to complete the reaction. Add 0.5 g of cefuroxime sodium seed crystals, add 950 ml of ethanol dropwise after 20 minutes of constant temperature. Then, the temperature was lowered to 0°C and kept constant for 1h. Suction filtration, ethanol washing, 20°C, vacuum degree of 0.1MPa and drying for 2 hours to obtain cefuroxime sodium product. The color grade of the product is lower than Y1 or YG1, the purity is 99.5%, and the yield is 93.7%.

Embodiment 3

[0023] Add 70ml of acetone and 20ml of pure water into the crystallizer, add 9g of cefuroxime acid, and stir at 30°C until fully dissolved. Add 8.9 ml of sodium isooctanoate aqueous solution with a concentration of 0.4 g / ml to the cefuroxime acid solution, and stir at constant temperature for 20 minutes to complete the reaction. Add 0.54 g of cefuroxime sodium seed crystals, keep the temperature constant for 15 minutes, and then add 450 ml of acetone dropwise. Then, the temperature was lowered to 2°C and kept constant for 1.5h. Suction filtration, acetone washing, 30°C, vacuum degree 0.09MPa and drying for 1.8 hours to obtain cefuroxime sodium product. The color grade of the product is lower than Y2 or YG2, the purity is 99.5%, and the yield is 92.1%.

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Abstract

The invention relates to a method utilizing coupling reaction crystallization to prepare cefuroxime sodium, which comprises dissolving cefuroxime acid in a mixed solvent at 20-30 DEG C to prepare a solution with the concentration to be 0.025g / ML-0.1g / Ml; adding an alkaline sodium salt water solution into the solution; mixing for 10-20min at constant temperature to enable a reaction to be complete, and adding cefuroxime sodium seed crystal; adding an elution agent after 10-20min; cooling the temperature of the solution to 0-5 DEG C, and keeping at the constant temperature for 0.5-2h; filtering, washing and drying the obtained suspension, and obtaining a cefuroxime sodium product. The method reduces the adsorption filtration process of activated carbon and avoids loss of yield. The method achieves coupling of reactions and crystallization, and the methods of elution crystallization and cooling crystallization are combined with each other in the crystallization process, the crystallization process is controlled easily, the particle size of the product is uniform, the liquidity is greatly improved, the purity is higher than 99.5%, and the yield is over 92%.

Description

Technical field [0001] The invention belongs to the technical field of crystallization, and particularly relates to a method for preparing cefuroxime sodium by coupling reaction crystallization of antibiotic drugs. Background technique [0002] Cefuroxime sodium belongs to the β-lactam antibiotics. It is the best second-generation cephalosporin with the advantages of the first and third-generation cephalosporins. It not only has strong antibacterial activity against gram-positive cocci, but also It also has good antibacterial activity against certain gram-negative bacteria, especially in the treatment of mixed infections of gram-positive and gram-negative bacteria, it is the preferred drug. Cefuroxime sodium is not metabolized by the liver in the body, so it is not toxic to the liver; it is excreted from the urine through the kidneys in its original form, so it has almost no toxic side effects to the kidneys, so its medication is very safe and has good pharmacokinetics for newbor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34
Inventor 王静康赵颖颖侯宝红黄权华尹秋响苏军权张美景杨战鏖王永莉龚俊波
Owner TIANJIN UNIV
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