Crystallization method of cephalosporanic acid

A cephalosporanic acid and crystallization technology, which is applied in the field of preparation of pharmaceutical and chemical raw materials, can solve the problems affecting the quality and poor quality of the final synthetic product, and achieve the effect of strong applicability and good crystal quality

Inactive Publication Date: 2012-01-18
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cephalosporanic acid crystals prepared by the existing crystallization method

Method used

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  • Crystallization method of cephalosporanic acid
  • Crystallization method of cephalosporanic acid
  • Crystallization method of cephalosporanic acid

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0013] Example 1

[0014] Measure 1000ml of cephalosporan acid to be crystallized with a concentration of 15-25mg / ml. At 20-30°C, add 1 g of sodium bisulfite, stir for 30 minutes, and add 5 ml of triethylenetetramine. Stir, add hydrochloric acid with a mass ratio of 15% to pH 6.2 to 6.3, continue stirring until crystals appear. Cultivate the crystal for 30 minutes, and continue to add hydrochloric acid with a mass ratio of 15% until the pH of the liquid to be crystallized is 4.2-4.4. Cultivate the crystals for 30 minutes, reduce the temperature to 0~5℃, and filter under vacuum. Wash it twice with 100ml of water at 0~1℃, and then wash it three times with 150ml of acetone at 0~1℃. The material is discharged and dried in a vacuum drying oven at 38-40°C under -0.098Mpa pressure for 3 to 5 hours.

Example Embodiment

[0015] Example 2

[0016] Measure 1000ml of cephalosporan acid to be crystallized with a concentration of 15-25mg / ml. Add 1ml of triethylenetetramine. Stir, add hydrochloric acid with a mass ratio of 18% until crystals are precipitated. After cultivating the crystals for 30 minutes, continue to add hydrochloric acid with a mass ratio of 18% until the pH of the solution to be crystallized is 4.2-4.4. Cultivate the crystals for 30 minutes, reduce the temperature to 0~5℃, and filter under vacuum. Wash twice with water and three times with acetone. Discharge and dry in vacuum.

Example Embodiment

[0017] Example 3

[0018] Measure 1000 ml of cephalosporan acid to be crystallized, add 2 g of sodium bisulfite under normal temperature conditions, stir for 20 minutes, and add 3 ml of triethylenetetramine. Stir, add hydrochloric acid with a mass ratio of 12% to pH 6.2-6.3, and continue to stir until crystals appear. Cultivate the crystals for 60 minutes, then add 15% hydrochloric acid by mass ratio until the pH of the liquid to be crystallized is 4.2-4.4. Cultivate the crystals for 20 minutes, lower the temperature to 0-5°C, vacuum filter, and wash the filtered crystals twice with cold water and twice with acetone. Discharge and dry in a vacuum drying oven.

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Abstract

The invention discloses a crystallization method of cephalosporanic acid, and the method comprises the following steps: (a) adding triethylenetetramine with a volume ratio of 1-5 parts per thousand into cephalosporanic acid liquid to be crystallized, slowly adding 12-18% by mass of hydrochloric acid till crystals are precipitated; (b) growing the crystals for 20-60 minutes; (c) adding 12-18% by mass of hydrochloric acid for the second time, when the pH of the liquid to be crystallized is 4.0-4.4, growing the crystals again for 20-60 minutes; (d) cooling to 0-5 DEG C, performing vacuum filtration, washing and drying the filtered crystals. The cephalosporanic acid crystals prepared by the method of the invention have good quality, and strong applicability.

Description

[0001] Field [0002] The present invention relates to the preparation method of pharmaceutical chemical raw materials, in particular to the crystallization method of 7-aminocephalosporanic acid. Background technique [0003] 7-Aminocephalosporanic acid (7ACA) is the starting material for many semi-synthetic cephalosporins. The current process of producing 7ACA usually adopts biological fermentation and chemical extraction to produce Cephalosporin C, then chemically cracks or enzymolyzes Cephalosporin C to generate a cephalosporanic acid solution, and then adds crystallization aids (such as polytetramine, acetone, etc.) to the solution. ), crystallized, and then washed and dried to obtain cephalosporanic acid crystals. The quality of cephalosporanic acid crystals prepared by the existing crystallization method is poor, which also affects the quality of the final synthetic product. Contents of the invention [0004] The object of the present invention is to provide a new cr...

Claims

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Application Information

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IPC IPC(8): C07D501/18C07D501/12
Inventor 孙燕程俊山张锁庆侯红杰杨梦德郭西峰闫峰蒋晓声徐更王新辉曹欢单晓丽段素英张苗静马金玉薛百庆郑宝丽米建伟姚振勇郭文仿王树林赵伟周文江
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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