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Method of synthesizing cefixime intermediate GVNE

A synthetic method, the technology of cefixime, which is applied in the field of cefixime, can solve the problems of low yield, high cost, and difficulty in solvent recovery, and achieve the effects of improving recycling rate, reducing material loss, and reducing production cost

Inactive Publication Date: 2007-08-15
河源市制药工程技术研究开发中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] As can be seen from the above: this process uses a variety of solvents, the composition of the mother liquor is more complicated, which is not conducive to recovery and reuse, and the yield of the final product is between 72% and 74%. The cost of synthesizing GVNE by this method is relatively high. Not only the yield is low, but also the solvent recovery is difficult

Method used

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  • Method of synthesizing cefixime intermediate GVNE

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Add 420L of dichloromethane and 88L of N,N-dimethylformamide into a dry reaction tank with an adjustable rotation speed with a nitrogen device, cool down to 5°C with nitrogen, add 80kg of GCLE, 24.2kg of three Phenylphosphonium, 8kg sodium iodide, maintain the temperature at 10°C with nitrogen gas, stir for 90 minutes, and carry out the phosphine salt reaction;

[0029] (2) After the reaction is complete, add 40L of 37% formaldehyde and cool to 5°C;

[0030] (3) Feed 160L of 1mol / L NaOH within 20 minutes, maintain the temperature at 5°C and continue stirring for 60 minutes to carry out the witting reaction;

[0031] (4) Prepare 500L 0.1mol / L HCl in a reaction tank with a liquid separation sight glass in advance, put the reaction pressure into the tank after the reaction, extract for 20 minutes, and let stand for 20 minutes;

[0032] (5) Liquid separation, the organic phase is transferred to another reaction tank with a liquid separation sight glass and variable spe...

Embodiment 2

[0039] (1) Add 532L of chloroform and 110L of N,N-dimethylformamide into a dry reaction tank with adjustable rotational speed with a nitrogen device, cool down to 10°C with nitrogen, add 100kg of GCLE, 30.2kg of three Phenyl phosphorus, 10kg potassium iodide, maintain the temperature at 15°C with nitrogen gas, stir for 60 minutes, and carry out the phosphine salt reaction;

[0040] (2) After the reaction is complete, add 50L of 37% formaldehyde and cool to 10°C;

[0041] (3) Feed 195L of 1mol / L KOH within 30 minutes, maintain the temperature at 10°C and continue stirring for 30 minutes to carry out the witting reaction;

[0042] (4) Prepare 600L 0.1mol / L HCl in advance in a reaction tank with a liquid separation sight glass. After the reaction, put the reaction liquid into the tank, extract for 30 minutes, and let stand for 30 minutes;

[0043] (5) Liquid separation, the organic phase is transferred to another reaction tank with liquid separation sight glass and variable spee...

Embodiment 3

[0050] (1) Add 480L of dichloromethane and 99L of N,N-dimethylacetamide into a dry reaction tank with an adjustable rotation speed with a nitrogen device, cool down to 8°C with nitrogen, add 90kg of GCLE, 27.2kg of three Phenylphosphonium, 9kg sodium iodide, maintain the temperature at 13°C with nitrogen gas, stir for 75 minutes, and carry out the phosphine salt reaction;

[0051] (2) After the reaction is complete, add 45L of 37% formaldehyde and cool to 8°C;

[0052] (3) Add 1mol / L KOH 175L within 25 minutes, maintain the temperature at 8°C and continue stirring for 45 minutes to carry out the witting reaction;

[0053] (4) Prepare 550L 0.1mol / L HCl in advance in a reaction tank with a liquid separation sight glass, put the reaction pressure into the tank after the reaction, extract for 25 minutes, and let stand for 25 minutes;

[0054] (5) Liquid separation, the organic phase is transferred to another reaction tank with liquid separation sight glass and variable speed stir...

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Abstract

The invention discloses a synthesizing method of cefuroxime intermediate, which is characterized by the following: adopting dichloromethane or trichloromethane solvent to react; fitting for recycling mother liquid; reducing cost; decompressing; distilling until the mass becomes viscous; adding carbinol to evolve; decompressing and distilling; extracting through dichloromethane or trichloromethane; reducing the loss of material; improving the recycling rate of solvent and receiving rate of product by 6-8%.

Description

technical field [0001] The invention belongs to the technical field of cefixime, in particular to a synthesis method of cefixime intermediate GVNE. Background technique [0002] Cefixime is a third-generation oral cephalosporin antibiotic, which has a broad-spectrum antibacterial effect on Gram-positive and Streptococcus), pneumococcus and Escherichia coli, Moraxella, Neisseria gonorrhoeae, Proteus mirabilis, and Cathaeria in Gram-negative bacteria showed stronger bactericidal effect than other oral cephalosporins. It has the characteristics of broad spectrum, high efficiency, enzyme resistance and low toxicity, and is an anti-infection oral drug widely used in clinical practice. [0003] The necessary stage for the production of cefixime is the synthesis of the cefixime intermediate GVNE. The current technical status of the synthesis of the cefixime intermediate GVNE is as follows: [0004] (1) Add GCLE, sodium iodide, triphenylphosphine, acetone, DMF (N,N-dimethylformami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22
Inventor 潘行远
Owner 河源市制药工程技术研究开发中心