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A kind of preparation method and composition of original developed quality cephradine

A technology of cephradine and composition, which is applied in the field of preparation of the original developed quality cephradine, can solve problems such as potential safety hazards, harsh reaction conditions, combustion and explosion, etc., and achieves the effects of simple and easy preparation method, low raw material cost, and avoiding degradation

Active Publication Date: 2018-07-10
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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  • A kind of preparation method and composition of original developed quality cephradine
  • A kind of preparation method and composition of original developed quality cephradine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 (preparation of cefradine)

[0029] (1) Add 100g of 7-ADCA, 500ml of dichloromethane, blow in nitrogen, stir, add 120ml of N-methylacetamide, heat to 45°C, add slowly and then slowly add 90g of 1,8-diazabicyclo[ 5,4,0] Undec-7-ene, constant temperature reflux reaction for 1.5 to 2 hours to obtain 7-ADCA protected by DBU;

[0030] (2) Add 120g of dihydrophenylglycine acid chloride hydrochloride to 300ml of dichloromethane, cool down to -20°C~-30°C; slowly add 7-ADCA protected by DBU at 0°C, and keep it at -5°C~ -10℃, condensation reaction for 2 hours;

[0031] (3) Add 500ml of water to the hydrolysis tank, cool to 2°C, add the reaction solution after the condensation reaction in the previous step and 140ml of concentrated hydrochloric acid into the hydrolysis tank, stir at 10°C for 15min, let stand, separate the organic phase layer and wait Use; Aqueous layer is heated to 38 ℃ rapidly, distills under vacuum condition simultaneously, to go out residual dich...

Embodiment 2

[0033] Embodiment 2 (the recovery of cephradine)

[0034] Combine the organic phase layer and the filtrate in Example 1, pass the combined solution through a 0.45 μm microporous filter membrane, then pump it into a polyamide membrane device for processing, first concentrate to 65% to 75% of the original volume of the combined solution, 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 the concentrated solution 1, and the permeate is ready for use;

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

[0036] Concentrate 1 and concentrate 2 are combined, and cephradine is extracted by β-naphthol complexation.

Embodiment 3

[0037] Embodiment 3 (preparation of composition)

[0038] Get L-arginine, the cephradine prepared by embodiment 1, by weight, according to the proportioning of 400 parts of L-arginine, 1000 parts of cephradine, place in water for injection, stir and make it dissolve. Spray drying in QZR-5 spray dryer, inlet temperature 105℃~115℃, outlet temperature 50℃~55℃, feed rate 25~40ml / min, nozzle pressure 0.25~0.40kgf / cm 2 , collect and mix powder with the cyclone separator to get the finished product. Get the finished product, pack in subpackages of 0.765 grams (equivalent to 0.5 grams of cephradine), crimp and pack afterwards to get final product.

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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 original-developed quality cephradine. Background technique [0002] Cephradine is the first generation of cephem-like β-lactam antibiotics for injection or oral administration. Pneumococci, Escherichia coli, and some Proteus 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 tissues. [0003] The original research company of cephradine is Bristol-Myers Squibb. According to the US FDA Orange Book database, the approval time is 1982.01.01. [0004] At present, the production of cephradine bulk drug mainly includes chemical synthesis and enzymatic synthesis. [0005] The enzymatic synthesis is a reaction catalyz...

Claims

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Application Information

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Patent Type & Authority Patents(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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