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Method for improving quality of cemandil sodium by using three-dimensional column plate to purify solvent

A technology of cefamandole sodium and three-dimensional trays is used in organic chemistry, pharmaceutical formulations, medical preparations containing active ingredients, etc., to achieve the effects of improving reaction quality and product quality, high product quality, and increasing solubility

Active Publication Date: 2017-04-19
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the research process of cefamandole sodium and its serial production, a large amount of organic solvents or even mixed organic solvents are used, so the quality of the organic solvent is very important to the impact of cefamandole sodium. At present, there is a lack of a purified organic solvent and mixed organic solvents. Technical methods for organic solvent purification

Method used

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  • Method for improving quality of cemandil sodium by using three-dimensional column plate to purify solvent
  • Method for improving quality of cemandil sodium by using three-dimensional column plate to purify solvent
  • Method for improving quality of cemandil sodium by using three-dimensional column plate to purify solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0042] ①Purification of solvent: Purify the mixed organic solvent with three-dimensional tray mass transfer technology;

[0043] ②Silylation reaction: Add 30g of 7-TMCA to a 1000ml reaction bottle in sequence, add 340ml of purified dichloromethane-chloroform mixed solvent and 20ml of hexamethyldisilica in a mass ratio of 95:5 Amine, the temperature is 15°C, reflux reaction for 1.5h until the system is clear, and the temperature is lowered to -5°C to obtain the reaction solution 1;

[0044] 3. the synthesis of cefamandoleate: add 14mlN in the above-mentioned reaction solution, N-dimethylaniline, slowly add 18mlD-formyl mandelic acid chloride and 25ml, the dichloromethane-trichloromethane that mass ratio is 95:5 solution, the system was reacted at a constant temperature of -5°C for 4.5 hours to obtain reaction solution 2;

[0045] ④Extraction: When the residual amount of 7-TMCA is less than 1%, add 200ml of water at a temperature of 18-20°C, control the temperature at 13-15°C a...

Embodiment 2

[0049] ①Purification of solvents: Purify mixed organic solvents with high-throughput and high-efficiency three-dimensional mass transfer tray technology;

[0050] ②Silylation reaction: Add 30g of 7-TMCA to a 1000ml reaction bottle in turn, add 330ml of purified dichloromethane-chloroform mixed solvent and 20ml of hexamethyldisilica in a mass ratio of 95:5 Amine, the temperature is 17°C, reflux reaction for 1h until the system is clear, and the temperature is lowered to -5°C to obtain the reaction solution 1;

[0051] 3. the synthesis of cefamandoleate: add 14mlN in the above-mentioned reaction solution, N-dimethylaniline, slowly add 18mlD-formyl mandelic acid chloride and 25ml, the dichloromethane-trichloromethane that mass ratio is 95:5 solution, the system was reacted at a constant temperature of -2°C for 4.5 hours to obtain a reaction solution 2;

[0052] ④Extraction: When the residual 7-TMCA is less than 1%, add 200ml of water at a temperature of 13-15°C, control the temp...

Embodiment 3

[0056] ①Purification of solvents: Purify mixed organic solvents with high-throughput and high-efficiency three-dimensional mass transfer tray technology;

[0057] ②Silylation reaction: Add 30g of 7-TMCA to a 1000ml reaction bottle in turn, add 300ml of dichloromethane-trichloromethane mixed solvent and 20ml of hexamethyl dichloromethane at a mass ratio of 95:5 Silicon amine, the temperature is 20°C, reflux reaction for 1.5h until the system is clear, and the temperature is lowered to -5°C to obtain the reaction solution 1.

[0058] 3. The synthesis of cefamandoleate: add 14mlN, N-dimethylaniline, slowly add 18mlD-formylmandelic acid chloride and 25ml, the solution of dichloromethane-trichloromethane that mass ratio is 95:5, system constant temperature React at -2°C for 5 hours to obtain reaction solution 2;

[0059] ④Extraction: When the residual amount of 7-TMCA is less than 1%, add 200ml of water at a temperature of 13-15°C, control the temperature at 13-15°C and stir for 3...

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Abstract

The present invention discloses a method for improving the quality of cemandil sodium by using a three-dimensional column plate to purify a solvent. The method comprises: solvent purification, alkylation reaction, cefamandole ester synthesis, extraction, cemandil sodium synthesis, and sterile sub-packaging. According to the present invention, during the cemandil sodium preparation process, the reaction system solvent is purified by using the high-throughput efficient three-dimensional mass transfer column tray technology so as to finally improve the quality of the cemandil sodium product and ensure the quality of the cemandil sodium powder-needle preparation for injection. The invention provides the method for improving the quality of the cemandil sodium powder-needle preparation for injection by using the three-dimensional column tray mass transfer technology to purify the organic solvent.

Description

technical field [0001] The invention relates to a method for improving the quality of cefamandole sodium by using three-dimensional trays to purify solvents, and belongs to the field of preparation of raw materials. Background technique [0002] Cefamandole sodium, as a relatively large variety of cephalosporins, currently has a huge market potential. This product is a second-generation cephalosporin antibiotic. Its structural formula is: [0003] The chemical name of this product is: (6R, 7R)-7(R)-(2-formyloxy-2-phenylacetamido]-3[[(1-methyl-1H-tetrazol-5-yl) )Thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt. Calculated as anhydrous matter, containing cefamen More (C18H17N6NaO6S2) 84.0% to 93.0%. [0004] This product can usually be used for infections caused by anaerobic bacteria, Gram-positive bacteria, and Gram-negative bacteria. Pseudomonas, Acinetobacter, and most Serratia species are resistant to cefamandole and some cephalospo...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04C07D501/12A61K9/14A61K31/546A61P31/04
CPCA61K9/0019A61K9/14A61K31/546C07D501/04C07D501/12C07D501/36
Inventor 胡利敏孙燕张锁庆杨梦德张文胜李敏柳世萍贾全刘萍胡少华
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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