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Method for preparation of fine cefamandole nafate

A technology of cefamandole sodium and organic sodium, applied in the direction of organic chemistry, etc., can solve the problems of complicated operation, cumbersome post-processing, restrictions, etc., and achieve the effects of easy quality control, good product stability, and easy operation.

Inactive Publication Date: 2012-10-03
SHANDONG LUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are complicated in operation and cumbersome post-processing, etc., which are greatly restricted in large-scale production.

Method used

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  • Method for preparation of fine cefamandole nafate
  • Method for preparation of fine cefamandole nafate
  • Method for preparation of fine cefamandole nafate

Examples

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Embodiment 1

[0021] Embodiment 1, refining cefamandole sodium

[0022] In 500mL four-necked flask, add cefamandole sodium crude product (purity is 97.6%) 35.0 grams, anhydrous salt 50g, organic solvent 1. acetone 245g and sodium isooctanoate 1.5g, stir to dissolving clear, control final pH value is 5.5, After controlling the temperature at 15°C, add 1.5g of activated carbon, stir for 0.5 hours, and filter with suction, transfer the obtained filtrate into a 2000mL four-neck flask, stir and add 700g of organic solvent ②Isopropanol until mixed, during which the temperature is controlled at 15°C, and crystals are precipitated , crystal growth, suction filtration, washing with organic solvent 2. isopropanol, and vacuum drying at 45° C. to obtain 32.1 g of white cefamandole sodium crystals provided by the present invention, with a yield of 91.7% and a purity of 99.6%. The structural confirmation data of the product are as follows figure 2 shown, with figure 1 Standard infrared spectrogram con...

Embodiment 2

[0024] Embodiment 2, refining cefamandole sodium

[0025] Add crude product cefamandole sodium (purity is 97.4%) 7.5kg, anhydrous salt 10.5kg, organic solvent 1. acetone 52.5kg and sodium isooctanoate 0.32kg in 100L enamel tank, stir until dissolving clear, control final pH value is 5.5 , after controlling the temperature to 5°C, add 310 g of activated carbon, stir for 0.5 hour, and filter with suction. Transfer the filtrate into a 500L enamel tank, stir and add 150kg of organic solvent ② isopropanol until well mixed, during which the temperature is controlled at 15°C, crystals are precipitated, crystals are grown, filtered with suction, washed with organic solvent ② isopropanol, vacuum dried at 45°C, Obtain 6.83 kg of white cefamandole sodium crystals provided by the present invention, with a yield of 91.1% and a purity of 99.7%.

[0026] The structural confirmation data of the product are as follows image 3 shown, with figure 1 The comparison shows that the structure of ...

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Abstract

The invention discloses a method for preparation of fine cefamandole nafate, comprising the steps of mixing crude cefamandole nafate with organic sodium salt, salt-free water and organic solvent (1); controlling pH value of the reaction system to 5.5-7.5 and reaction temperature to 5-15 DEG C; adding active carbon and then filtering to obtain filtrate; mixing the filtrate with organic solvent (2) and separating out crystal to obtain the cefamandole nafate. The method for preparation of the fine cefamandole nafate provided by the invention overcomes the disadvantages of prior preparation method, and has the advantages of simple operation, short preparation period, easy quality control, good product stability and important application value.

Description

technical field [0001] The invention relates to a method for refining cefamandole sodium. Background technique [0002] Cefamandole Nafate (Cefamandole Nafate) is the second generation of semi-synthetic cephalosporin developed by Eli Lilly and Company in 1972. It was used clinically in 1978. Its trade name is Mandol, and its chemical name is 7-D-(2- Formyloxyphenylacetamide)-3-[(1-methyl-1H-tetrazol-5 base)thiomethyl]-3-cephem-4-carboxylic acid sodium salt, the molecular weight is 512.50, and its structural formula is as follows I show: [0003] [0004] Formula I [0005] The synthetic method of cefamandole sodium is reported in many periodicals at home and abroad: patents such as US4351947, EP0432297, CN101475580A, these methods can effectively prepare cefamandole sodium, but the purity of the target product is not high, the color is poor, and the content is low. For this reason, there are also research and development patents for the refining process of cefamandole ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
Inventor 王小丹翟昌梅张淑婷张冬梅陈君
Owner SHANDONG LUKANG PHARMA
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