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A kind of method of solid phase synthesis cefotaxime

A technology for cefotaxime and solid-phase synthesis, which is applied in the direction of organic chemistry, etc., can solve the problems of low total yield of cefotaxime, complicated operation, low purity, etc., and achieves improved total reaction yield, simplified reaction procedure, and product purity. improved effect

Active Publication Date: 2021-02-26
SHANGHAI NEW ASIA PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at overcoming above-mentioned defect, provides a kind of method for solid-phase synthesis of cefotaxime, solves the technical problems of low total yield, low purity and complicated operation in the preparation process of cefotaxime in the prior art

Method used

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  • A kind of method of solid phase synthesis cefotaxime
  • A kind of method of solid phase synthesis cefotaxime
  • A kind of method of solid phase synthesis cefotaxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Bridging of 7-ACA and solid phase carrier

[0018]

[0019] In the glazed glass column, react 25g 7-ACA and chloromethyl resin in 100ml DMF, make it fully bridged with the solid-phase carrier, use N after the end of the reaction Flow to remove the solvent, wash the resin with dichloromethane and pyridine, Proceed directly to the next reaction.

Embodiment 2

[0020] Embodiment two: prepare the cefotaxime of solid phase bridging

[0021]

[0022] In a glazed glass column, then add dichloromethane (75ml)-triethylamine (8g) solution in the column, stir under nitrogen protection, add 25g 2-(2-amino-4-thiazolyl)-2 at room temperature -(methoxyimino) thiothiazolyl acetate, react for 6h. After the reaction, the solvent was removed under N2 flow, and the resin was washed with dichloromethane and pyridine.

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Abstract

The invention is applicable to the field of chemical pharmaceutical preparation, and provides a method for preparing cefotaxime through a solid-phase synthetic method. The method comprises the steps of bridging connection of raw material 7-ACA and a solid phase, solid phase synthesis and a separation reaction of a product and the solid phase. The preparation method for the cefotaxime provided by the invention avoids the steps such as post-treatment, purification and drying in the reaction process, greatly simplifies the reaction operation, reduces impurities in the reaction process, and improves the production benefits and the product quality.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, in particular to a preparation method of cefotaxime. Background technique [0002] Cefotaxime, the chemical name is (6R,7R)-3-[(acetyloxy)methyl]-7-[[(2-amino-4-thiazolyl]-(methoxyimino)acetyl]amino ]-8-Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, the structural formula is: [0003] [0004] Cefotaxime is the third-generation cephalosporin, which is widely used clinically to treat sepsis caused by sensitive bacteria, suppurative meningitis and respiratory tract, urinary tract, biliary tract, bone and joint, skin and soft tissue, abdominal cavity, digestive tract, facial features, Infection of the genitals and other parts. [0005] In the existing literature, the preparation process of cefotaxime is divided into two steps. 7-ACA and AE-active ester are reacted in dichloromethane under the action of amine compounds, then acidified by adding hydrochloric acid, and then cooled to c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/34
CPCC07D501/34
Inventor 胡国栋崔万胜商鼎
Owner SHANGHAI NEW ASIA PHARMA
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