Preparation method of cefazolin sodium

A technology of cefazolin sodium and cefazolin, which is applied in the field of preparation of pharmaceutical compounds, can solve the problems of environmental pollution, complicated process, and low yield, and achieve the effects of high recovery rate, simple process, and simple recovery

Active Publication Date: 2012-01-18
哈药集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The above methods are complex in process, difficu

Method used

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

Examples

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Embodiment 1

[0041] Step 1, three-position intermediate (TDA) of cefazolin sodium is synthesized

[0042] 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.

[0043] Step 2, cefazolin acid synthesis

[0044] 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 invention relates to the preparation of a pharmaceutical compound, in particular to the preparation of cefazolin sodium. Background technique: [0002] Cefazolin Sodium [0003] English name: Cefazolin Sodium (Cefamezin) [0004] Alias: Pioneermycin Ⅴ, cephalosporin Ⅴ, cephalosporin, cifazoline, cephalosporin oxazoline, cephalosporin, Kaifuzhuo, Pioneer 5. [0005] Chemical name: (6R,7R)-3-[[(5-methyl-1,3,4-thiadiazol-2-yl)sulfur]methyl]-7-[(1H-tetrazole-1- Base) Acetylamino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt. [0006] Molecular formula: C14H13N8NaO4S3. [0007] Molecular weight: 476.48. [0008] Properties: White or off-white crystalline powder, almost odorless, bitter taste. 1.05g of this product is approximately equivalent to 1g of cefazolin base. 1g of this product contains about 2.1mmol (2.1mEq) of sodium ion. [0009] This product is easily soluble in water, and the pH value of 10% aqueous soluti...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04C07D501/12
Inventor 吴志军余威杨新春陶树青
Owner 哈药集团股份有限公司
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