Preparation method of cefodizime sodium

A technology of cefodizime sodium and compounds, which is applied in the field of chemical drug synthesis, can solve the problems of high polymer content and short synthesis reaction steps, and achieve the effects of high product yield, low product cost and time saving

Active Publication Date: 2012-12-12
AMICOGEN CHINA BIOPHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] For the deficiencies in the prior art, the object of the present invention is to provide a kind of method that replaces traditional 7-ACA with GCLE as starting material to prepare cefodizime sodium, and synthesize cefodizime sodium in two steps with GCLE, which solves the existing problem There is a problem of high polymer content in the technology, the synthesis reaction steps are short, the side reactions are few, the operation is simple, the yield is high, and the product obtained is high in purity

Method used

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  • Preparation method of cefodizime sodium
  • Preparation method of cefodizime sodium
  • Preparation method of cefodizime sodium

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Effect test

Embodiment 1

[0034] The preparation method of cefodizime sodium adopts compound I as a starting material, and the specific steps include:

[0035] (1) Add 30g of compound I (GCLE) and 12.3g of compound II into a system containing 200mL of acetone and 20mL of water, heat to 50°C, stir until clear, add 0.3g of sodium iodide, and use a mass fraction of 10% sodium carbonate Adjust the pH of the solution to 5.0, react for 2 hours, add 100 g of trifluoroacetic acid for hydrolysis, add 1.5 g of activated carbon for decolorization, wash with a mixture of 10 mL of acetone and 1 mL of water, adjust the pH to 3.0 with 25% ammonia water, and culture at 10 °C. crystallize for 1 hour, filter with suction, wash with 100mL of water and 100mL of acetone respectively, and dry in vacuo to obtain 22.1g of compound III with a yield of 92% and a purity of 98.76%;

[0036] (2) Add 20g of compound III and 27.4g of compound IV into a mixed solvent system containing 100mL of toluene and 100mL of methanol, dropwise ...

Embodiment 2

[0039] The preparation method of cefodizime sodium adopts compound I as a starting material, and the specific steps include:

[0040] (1) Add 30g of compound I (GCLE) and 13.2g of compound II into a system containing 200mL of acetone and 15mL of water, heat to 50°C, stir until clear, add 0.7g of sodium bromide, and use a mass fraction of 8% bicarbonate Adjust the pH to 5.5 with sodium solution, react for 1 hour, add 141g of trifluoroacetic acid for hydrolysis, add 1.5g of activated carbon for decolorization, wash with 10mL of acetone and 0.75mL of water mixture, adjust the pH to 3.5 with 28% ammonia water, 12°C Cultivate the crystal for 1 hour, filter with suction, wash with 100 mL of water and 100 mL of acetone respectively, and dry in vacuo to obtain 21.8 g of compound III with a yield of 91% and a purity of 98.62%;

[0041] (2) Add 20g of compound III and 34.2g of compound IV into a mixed solvent system containing 200mL of toluene and 100mL of ethanol, add dropwise 23mL of ...

Embodiment 3

[0044] The preparation method of cefodizime sodium adopts compound I as a starting material, and the specific steps include:

[0045] (1) Add 30g of compound I (GCLE) and 14.1g of compound II into a system containing 200mL of acetone and 10mL of water, heat to 50°C, stir until clear, add 0.9g of potassium bromide, and use 12% carbonic acid Adjust the pH to 5.2 with sodium hydrogen solution, react for 2 hours, add 54 g of trifluoroacetic acid for hydrolysis, add 1.5 g of activated carbon for decolorization, wash with a mixture of 10 mL of acetone and 1 mL of water, adjust the pH to 3.5 with 26% ammonia water, and heat at 15 °C Cultivate the crystal for 1 hour, filter with suction, wash with 100 mL of water and 100 mL of acetone respectively, and dry in vacuo to obtain 21.5 g of compound III with a yield of 90% and a purity of 98.56%;

[0046] (2) Add 20g of compound III and 30g of compound IV into a mixed solvent system containing 100mL of acetone and 100mL of methanol, dropwis...

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Abstract

The invention relates to a preparation method of cefodizime sodium. By the preparation method, GCLE substitutes for traditional 7-ACA (7-Aminocephalosporanic acid) as starting materials to synthesize the cefodizime sodium, and after decoloration, reaction liquor is not subjected to separation and purification but is directly dropwise added with salt-forming agents for reaction so that the cefodizime sodium is obtained. The preparation method is short in step and less in side reaction, solves the problem of high superpolymer content of a final product and enables the superpolymer content to be decreased from 1.0% to smaller than 0.1%, product purity is improved and is above 99.8%, and product yield is improved and is above 90% by the aid of the raw material ratio and mixed solvent. Additionally, the preparation method is shorter in process step, timesaving, simple in process, high in yield and product purity, low in cost, cheap and available in raw materials and suitable for industrial production.

Description

Technical field [0001] Background technique [0002] 20 H 18 N 6 O 7 S 4 Na 2 [0003] [0004] [0005] [0006] quality. Invention content [0007] [0008] [0009] [0010] [0011] [0012] [0013] [0014] [0015] waste. [0016] [0017] [0018] [0019] [0020] [0021] [0022] [0023] 2 [0024] [0025] [0026] [0027]The preparation method of cephalosporine sodium sodium provided by the present invention has a short step and a small side reaction. It solves the problem of high high polymer content in the final product.The purity is more than 99.8%. The raw material ratio and the use of hybrid media have increased the income and make the product revenue of more than 90%.The present invention has shortened the process steps, saving time, simple process, high income, low cost, high product purity, cheap raw materials, and suitable for industrial production. Attachment description [0028] Attach figure 1 For the embodiment of the present invention 1 Cepait...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/06
Inventor 赵新祥王玲胡方锋张振安
Owner AMICOGEN CHINA BIOPHARM CO LTD
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