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Preparation method and composition of cefradine with original research quality

A technology for cefradine and a composition is applied in the field of preparation of cefradine of the original development quality, which can solve the problems of easy occurrence of potential safety hazards, harsh reaction conditions, difficult control and the like, and achieves a simple and easy preparation method, low cost of raw materials, and avoidance of yield reduction. Effect

Active Publication Date: 2016-06-29
广东金城金素制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, pivaloyl chloride is a dangerous chemical, flammable, and there is a danger of burning and explosion when exposed to open flames, high heat, or contact with oxidants. When heated or exposed to water, it releases heat and emits toxic and corrosive fumes. The reaction conditions for the synthesis of mixed anhydrides from salt and pivaloyl chloride are harsh, the reaction is violent, it is difficult to control, and it is easy to cause safety hazards

Method used

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  • Preparation method and composition of cefradine with original research quality
  • Preparation method and composition of cefradine with original research quality

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 (Preparation of Cefradine)

[0029] (1) Add 100g 7-ADCA, 500ml dichloromethane, pass nitrogen, stir, add 120ml N-methylacetamide, heat to 45°C, slowly add 90g 1,8-diazabicyclo[5,4 ,0]undec-7-ene, the constant temperature reflux reaction for 1.5 to 2 hours to obtain 7-ADCA silicone grease;

[0030] (2) Add 120g of dihydrophenylglycine acid chloride hydrochloride to 300ml of dichloromethane, cool down to -20℃~-30℃; slowly add 7-ADCA silicone grease at 0℃ dropwise, maintain -5℃~-10℃ , the condensation reaction is 2 hours;

[0031] (3) add 500ml of water to the hydrolysis tank, cool to 2°C, add the reaction solution after the previous step condensation reaction and 140ml of concentrated hydrochloric acid into the hydrolysis tank, stir at 10°C for 15min, stand, separate the organic phase layer and wait for Use; the water layer is rapidly heated to 38°C, and distilled under vacuum conditions at the same time to remove the residual dichloromethane; when the GC chro...

Embodiment 2

[0033] Example 2 (recovery of cefradine)

[0034] Combine the organic phase layer and the filtrate in Example 1, pass the combined liquid through a 0.45 μm microporous filtration membrane, and then pump it into a polyamide membrane device for treatment, first concentrate to 65% to 75% of the original volume of the combined liquid, and then Add 1-2 times the current volume of water, and then concentrate to 15% to 25% of the original volume of the combined solution to obtain concentrated solution 1, and the permeate is for later use;

[0035] The permeate is pumped into a polyamide membrane device for processing, and concentrated to 10% to 15% of the original volume of the permeate to obtain concentrated solution 2;

[0036] Concentrate 1 and concentrate 2 were combined, and cefradine was extracted by β-naphthol complexation.

Embodiment 3

[0037] Example 3 (Preparation of Composition)

[0038] Take L-arginine and the cefradine prepared in Example 1, by weight, according to the ratio of 400 parts of L-arginine and 1000 parts of cefradine, put them in water for injection, and stir to dissolve. Spray drying in QZR-5 type spray dryer, inlet temperature 105℃~115℃, outlet temperature 50℃~55℃, feed rate 25~40ml / min, nozzle pressure 0.25~0.40kgf / cm 2 , and the powder is collected and mixed with the cyclone separator to obtain the finished product. Take the finished product, pack it according to the sub-packaging volume of 0.765 g (equivalent to 0.5 g of cefradine), and then roll the lid and pack it.

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Abstract

The invention discloses a preparation method of cefradine with an original research quality on the basis of KR840002043 (B1) and US4235900 (A). The preparation method comprises steps as follows: (1) dihydrophenylglycine chloride hydrochloride is added to a solvent, the mixture is cooled, protected 7-ADCA is added to the mixture, and the mixture is subjected to a condensation reaction after being mixed; (2) water and hydrochloric acid are added after the reaction ends, the mixture is subjected to a hydrolysis reaction, an organic phase layer is left to stand for use, a water layer is subjected to vacuum distillation, and non-distillate is retained; (3) the non-distillate is crystallized and filtered, filtrate is left to stand for use, a filter cake is washed and dried, and cefradine is obtained; (4) the organic phase layer and the filtrate are combined, and cefradine is recycled and extracted. The invention further discloses composition of cefradine with the original research quality. The prepared cefradine and the cefradine composition have the original research quality, the preparation method is simple, the reaction conditions of the whole procedure are relatively mild, the cost of raw materials is low, little pollution is caused, and the prepared cefradine composition has stable and high quality.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method and composition of cefradine of the original development quality. Background technique [0002] Cefradine is the first-generation injection or oral cephem β-lactam antibiotic drug, the main drug has strong bactericidal effect on drug-resistant Staphylococcus aureus and Klebsiella pulmonary Pneumococcus, Escherichia coli, and some Proteobacteria all have antibacterial effects, and have the advantages of broad antibacterial spectrum, strong bactericidal power, small allergic reaction, and high stability to β-lactamase. Clinically, it is mainly used to treat infections of the respiratory tract, urinary tract, skin and soft tissue. [0003] The original research company of cefradine is Bristol-Myers Squibb. According to the US FDA Orange Book database, the approval date is 1982.01.01, the brand name is VELOSEF (Fanjiefu), and it is listed in China. [0004] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22C07D501/04C07D501/12A61K31/545A61K31/198A61P31/04
CPCA61K31/198A61K31/545C07D501/04C07D501/12C07D501/22A61K2300/00
Inventor 傅苗青赵叶青孙滨许蕾朱旭伟马庆双周白水王雷
Owner 广东金城金素制药有限公司
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