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Preparation method of catalyst for producing cephalosporin

A cephalosporin and catalyst technology, applied in the field of catalyst preparation, can solve the problems of only reaching 25%, difficult to control the dosage, yellowing, etc., and achieve the effects of increasing the content of active ingredients and stable performance

Active Publication Date: 2010-11-24
SHANDONG HEYI GAS CO LTD DONGYING CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low solubility of boron trifluoride acetonitrile complex in acetonitrile, the content of boron trifluoride in the saturated solution is only 10% at 25°C, and the current production process can only reach 25%
The boron trifluoride content is low, and it is difficult to control the amount added during use
Simultaneously because boron trifluoride of free state in acetonitrile is prone to photochemical reaction, the finished product color of low concentration can turn yellow, has influenced product quality and use effect, makes the yield of synthetic cefazolin reduce

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add sulfuric acid, boric acid, and hydrofluoric acid into the gas generator at a mass ratio of 6:1:1, and react at 125°C for 12 hours to form boron trifluoride gas. The gas in the gas-generating kettle enters the complexing kettle, and the complexing kettle is filled with acetonitrile. The mass ratio of the filling amount of acetonitrile to the boron trifluoride gas produced by each kettle in the gas-generating kettle is 6:1. The complexation temperature is 50°C and the time is 10 hours. When complexing, use a pump to circulate the acetonitrile solution in the complexing tank and the filter, and at the same time cool the filter so that the temperature in the filter is 16°C lower than the temperature in the complexing tank, so that the acetonitrile complex containing boron trifluoride The mother liquor of the compound becomes a supersaturated solution at this temperature, and crystals are precipitated;

[0018] The mother liquor is returned to the complexing kettle for ...

Embodiment 2

[0020] Add sulfuric acid, boric acid, and hydrofluoric acid into the gas generator at a mass ratio of 5:1:1, and react at 150°C for 15 hours to generate boron trifluoride gas. The gas from the gas-generating kettle enters the complexing kettle, and the complexing kettle is filled with acetonitrile. The mass ratio of the filling amount of acetonitrile to the boron trifluoride gas produced by each kettle in the gas-generating kettle is 5:1, and the complexing temperature is 58°C , the time is 8 hours. All the other are with embodiment 1. The finished product is white crystal, and the mass content of boron trifluoride reaches 50%.

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PUM

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Abstract

The invention discloses a preparation method of a catalyst for producing cephalosporin, comprising the following steps: (1) allowing sulfuric acid and boric acid to react with hydrofluoric acid to generate boron trifluoride gas; and (2) mixing the boron trifluoride gas with acetonitrile for complexation to obtain complexing mother liquor, then carrying out cooling crystallization, and collecting solid crystal from the complexing mother liquor to finally obtain the catalyst for producing the cephalosporin. In the invention, the boron trifluoride and acetonitrile complex obtained by the method is a white solid crystal which contains no less than 45% of boron trifluoride, and the complex has stable performances and multiplied content of effective ingredients in the product, thus overcoming the defects of the low-density product.

Description

technical field [0001] The present invention relates to a process for the preparation of catalysts for the production of cephalosporins. Background technique [0002] Cephalosporins are a series of semi-synthetic antibiotics obtained by modifying the side chain of cephalosporin C isolated from the culture solution of Cephalosporus coronaris. Its advantages are: wide antibacterial spectrum, high efficiency against anaerobic bacteria; lower allergic reaction than penicillins; more stable to acid and β-lactamase produced by various bacteria; same mechanism of action as penicillin, also inhibits bacterial cell wall formation to achieve the purpose of sterilization. It is a fungicide during breeding season. Because of its low adverse reactions and side effects, it is a class of antibiotics that are currently being developed rapidly. [0003] Boron trifluoride acetonitrile complex is a highly active catalyst for the synthesis of cephalosporin antibacterial drugs, and its effect...

Claims

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Application Information

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IPC IPC(8): C07F5/02B01J31/22C07D501/02
Inventor 于景东刘喜民张斌周士蒿
Owner SHANDONG HEYI GAS CO LTD DONGYING CITY