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A kind of cefuroxime lysine and preparation thereof

A technology for cefuroxime lysine and cefuroxime acid, which is applied in the preparation of cyanide reaction, the preparation of organic compounds, and medical preparations containing active ingredients, etc., can solve the problems of many impurities and low purity, and achieve high purity , the effect of strong stability

Active Publication Date: 2016-05-04
SHANDONG LUOXIN PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Then the impurity in the cefuroxime lysine crystal in the prior art is many, and purity is not high, for this reason, propose the present invention

Method used

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  • A kind of cefuroxime lysine and preparation thereof
  • A kind of cefuroxime lysine and preparation thereof
  • A kind of cefuroxime lysine and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 13

[0077] Example 13-Preparation of Decarbamoyl-Acetyl-Cefoxime Sodium:

[0078]

[0079] (1) Preparation of 7-aminocephalosporan acid crystals:

[0080] a-1. Weigh 7-aminocephalosporan acid and add 30 times the weight of water to form a suspension, add 4mol / l ammonia water, stir until the 7-aminocephalosporan acid is completely dissolved, and the pH of the solution is 6.8;

[0081] a-2. Add 4mol / l hydrochloric acid and an organic solvent, the organic solvent is a mixed solvent with a volume ratio of ethanol and ethyl acetate of 2:1, and the volume of the added organic solvent is 7-aminocephalosporan acid suspension 2 times the liquid volume; when the pH is 3.5, stop adding hydrochloric acid and continue adding organic solvents;

[0082] a-3. After the organic solvent is added, the crystals are grown for 2 hours, filtered, washed, and vacuum dried to obtain 7-aminocephalosporanic acid crystals. Its X-ray diffraction curve is like Figure 14 Shown

[0083] (2) Preparation of 7-ACA solution...

Embodiment 2

[0100] Example 2. Preparation of 3-decarbamoyl cefuroxime acid

[0101]

[0102] a. Measure 32ml of methanol, 18ml of NaOH solution (15%), stir and reduce the temperature to -16~-20℃, maintain at this temperature, dropwise add condensation solution and 6ml of water at 2℃; after the addition, maintain the temperature of the solution Stir for 15-20 minutes at -16~-20℃;

[0103] b. Add 5.4ml of glacial acetic acid dropwise and heat up the water bath. When the temperature of the solution reaches 5-10°C, add 0.10g of Sodium sulfonate and EDTA each, continue stirring, and then add 75ml of dichloromethane. At this time, The temperature will rise, and the pH of the solution will be between 5 and 6;

[0104] c. Add dropwise HCl solution (16%) 26ml, adjust the pH value of the solution to 2.0, then continue to stir for 30 minutes, reduce the temperature to 5°C, and maintain stirring for 30 minutes;

[0105] d. Filter, wash 3 times with water at 2°C, wash 2 times with dichloromethane, drain, and...

Embodiment 3

[0106] Example 3. Preparation of Cefuroxime Acid

[0107]

[0108] a. Add 85ml of anhydrous tetrahydrofuran to the reaction flask, cool to 1~4℃, add descarbamyl cefuroxime under nitrogen filling conditions, and stir until completely dissolved;

[0109] b. Cool the solution to -70°C, while continuing to cool down, add 5.2ml of chlorosulfonyl isocyanate (CSI) dropwise; after the addition, the solution temperature should not exceed -50~-45°C;

[0110] c. Quickly stir at -50~-45℃ for 30 minutes, add dropwise 18ml of 2℃ water, maintain the temperature of the solution at 0~5℃, and continue stirring for 10 minutes;

[0111] d. Add NaHCO to the reaction flask 3 Solution (NaHCO 3 18.00g+140ml of pure water heated to 35~40℃ and stirred to dissolve), adjust the pH value of the solution between 6.5~7.0;

[0112] e. After stirring for 10 minutes, add 72ml of ethyl acetate, stir thoroughly, the pH of the aqueous phase is ≈6;

[0113] f. The water bath is heated to 20°C, and 30% HCl solution is added d...

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Abstract

The invention relates to a cefuroxime lysine compound. The cefuroxime lysine contains 98-99.99% by weight of cefuroxime lysine and 0.01-2% of trans-cefuroxime acid, and the molecular formula of the trans-cefuroxime acid is as shown in formula I. The obtained cefuroxime lysine disclosed by the invention has very strong stability which is higher than that of the prior art; and the impurity content and the polymer content are lower than those of the cefuroxime lysine in the prior art, thus the cefuroxime lysine is very suitable for clinical applications.

Description

Technical field [0001] The invention relates to a pharmaceutical composition, in particular to a cefuroxime lysine and a preparation thereof. Background technique [0002] Cefuroxime belongs to the second-generation broad-spectrum cephalosporin drug. It was successfully developed by Glaxo Wellcome (now GlaxoSmithKline). It was first marketed in the UK, Ireland, Germany and Italy in 1978 under the trade name Xili Xin (Zinacef), subsequently sold in many countries around the world. It was approved by the US FDA on December 28, 1987, and was listed in the US in 1988. Due to its definite curative effect, wide antibacterial spectrum, low kidney toxicity, strong permeability, and stability to β-lactamase, it is widely used to combat various infections caused by sensitive bacteria. At present, cefuroxime has been included in "United States Pharmacopoeia 32nd Edition-NF27", "British Pharmacopoeia 2009 Edition", "Japanese Pharmacopoeia JP14 Edition", and "Chinese Pharmacopoeia 2010 Edit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/34C07D501/04C07C229/26C07C227/18A61K31/546A61P31/04
Inventor 李明华何雅官杨磊祥王永
Owner SHANDONG LUOXIN PHARMA GRP CO LTD
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