Preparation method of cefazolin sodium

A cefazolin sodium, condensation reaction technology, applied in the direction of organic chemistry, etc., to achieve the effect of less allergic phenomenon, reduce pollution, and improve quality

Active Publication Date: 2015-07-15
哈药集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The above methods are complex in process, difficult in operation, low in yield and pollute the environment

Method used

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  • Preparation method of cefazolin sodium
  • Preparation method of cefazolin sodium
  • Preparation method of cefazolin sodium

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Step 1, three-position intermediate (TDA) of cefazolin sodium is synthesized

[0043] Add 500g of dimethyl carbonate and 500g of boron trifluoride-dimethyl carbonate solution into the condensation reaction bottle and stir, then put 150g of thiadiazole and 300g of 7-ACA into the reaction bottle, and raise the temperature at the same time, the reaction temperature is 35-40°C , reacted until the residue of 7-ACA was less than 1.0%. After the reaction is complete, transfer the reaction solution into a crystallization bottle containing 3000ml of deionized water and 500ml, add ammonia water dropwise to pH 2-4, cool down to 10°C, and stir for 1 hour to grow crystals. Filter, wash the material with acetone until the material liquid is colorless and drain, and put the wet product into the next step.

[0044] Step 2, cefazolin acid synthesis

[0045] Add 80g of tetrazolium acetic acid to 1000ml of dichloromethane, cool down to -50±1°C, add 120ml of triethylamine dropwise within...

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PUM

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Abstract

The invention relates to a preparation method of a pharmaceutical compound, in particular relates to a preparation method of cefazolin sodium. The preparation method provided by the invention comprises the following steps: step 1, synthesizing TDA (toluene diamine); step 2, synthesizing cefazolin; and step 3, synthesizing cefazolin sodium.

Description

Technical field: [0001] The present invention involves the preparation of a pharmaceutical compound, which specifically involves the preparation of cephalizolin sodium. Background technique: [0002] Cephalipin sodium [0003] English name: CEFAZOLIN SODIUM (Cefamezin) [0004] Alias: Pionomycin V, Cefacin V, Pionorpin, Sytomoline, Polyoline Cobein, Pionein, Kay Fuzhuo, Pioneer 5. [0005] Chemical name: (6R, 7R) -3-[(5-methyl-1, 3, 4-噻 dioli-2-yl) sulfur] -7- [1H-tetrazol-1-Acetimamanamin group] -8-oxygen-5-sulfur-1-nitrogen miscellaneous two-ring [4.2.0] Xin-2-hydramel-2-sodium methampate salt. [0006] Molecular formula: C14H13N8NAO4S3. [0007] Molecular weight: 476.48. [0008] Properties: white or gray -white crystalline powder, almost odorless, bitter.This product 1.05g is equivalent to cephalopylene alkaline -based 1g.This product 1G contains about 2.1mmol (2.1Meq). [0009] This product is easy to dissolve in water, and the pH value of 10 % water solution is 4.5 to 6.Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/04C07D501/12
Inventor 王喜军余威杨新春陶树青
Owner 哈药集团股份有限公司
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