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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 are of poor quality, which also affects the quality of the final synthetic product

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
Effect test

Embodiment 1

[0014] Measure 1000ml of cephalosporanic acid liquid 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 concentration of 15% to pH 6.2-6.3, and continue stirring until crystals appear. After growing the crystal for 30 minutes, continue to add hydrochloric acid with a mass ratio concentration of 15%, until the pH of the liquid to be crystallized is 4.2-4.4. Cultivate the crystal for 30 minutes, cool down to 0-5°C, and vacuum filter. Wash twice with 100ml of water at 0-1°C, and then wash with 150ml of acetone at 0-1°C for three times. The material is discharged and dried in a vacuum drying oven at 38-40°C for 3-5 hours under the pressure of -0.098Mpa.

Embodiment 2

[0016] Measure 1000ml of cephalosporanic acid liquid to be crystallized, with a concentration of 15-25mg / ml. Add 1ml of triethylenetetramine. Stir, and add hydrochloric acid with a mass ratio concentration of 18% until crystallization occurs. After growing the crystal for 30 minutes, continue to add hydrochloric acid with a mass ratio concentration of 18%, until the pH of the liquid to be crystallized is 4.2-4.4. Cultivate the crystal for 30 minutes, cool down to 0-5°C, and vacuum filter. Wash twice with water and three times with acetone. The material was discharged and dried in vacuum.

Embodiment 3

[0018] Measure 1000ml of cephalosporanic acid liquid to be crystallized, add 2g of sodium bisulfite at room temperature, stir for 20 minutes, and add 3ml of triethylenetetramine. Stir, add hydrochloric acid with a mass ratio concentration of 12% to pH 6.2-6.3, and continue stirring until crystals appear. After growing the crystal for 60 minutes, add hydrochloric acid with a mass ratio concentration of 15%, until the pH of the liquid to be crystallized is 4.2-4.4. Crystal growth for 20 minutes, cooling to 0-5°C, vacuum filtration, washing the filtered crystal twice with cold water and twice with acetone. The material is discharged and dried in a vacuum 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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