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Preparation method of enoxacin gluconate

A technology of gluconic acid and enoxacin, which is applied in the field of preparation of enoxacin gluconate, can solve the problems of low reactivity, affecting product yield and quality, losing advantages in safety and cost, and improving yield. and quality, reduce the cost of preparation, and ensure the effect of safety

Inactive Publication Date: 2012-10-31
JIANGSU HI STONE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent scheme has the following deficiencies: first, due to the low reactivity of glucono-δ-lactone, it needs to be heated (50-60°C) for the reaction, but the heating reaction will affect the product yield and quality; Water and ethanol are used as solvents, so there is no advantage in safety and cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A) To prepare enoxacin gluconate solution, add gluconic acid to the purified water equipped with a stirring device and meet the standards of the Chinese Pharmacopoeia to dissolve the gluconic acid in the purified water, add enoxacin to stir and react, and then statically Put 8h, obtain enoxacin gluconate solution, in this step, the weight ratio of gluconic acid, purified water and enoxacin is 0.5: 8: 1, the temperature of described stirring reaction is 40 ℃, the reaction time 180min;

[0023] B) To prepare enoxacin gluconate crude product, first stir the enoxacin gluconate solution obtained in step A) again for 100 min, then filter, concentrate the filtrate under reduced pressure, and the reduced pressure is -0.8MPa, concentrate the concentrated solution to 1 / 4 of the volume of the enoxacin gluconate solution, the concentration temperature is 60°C, then cooling and crystallization, the cooling crystallization temperature is 0°C, suction filtration and drying, the dr...

Embodiment 2

[0026] A) To prepare enoxacin gluconate solution, add gluconic acid to the purified water equipped with a stirring device and meet the standards of the Chinese Pharmacopoeia to dissolve the gluconic acid in the purified water, add enoxacin to stir and react, and then statically Put 12h, obtain enoxacin gluconate solution, in this step, the weight ratio of gluconic acid, purified water and enoxacin is 1: 15: 3, the temperature of described stirring reaction is 20 ℃, the reaction time 480min;

[0027] B) To prepare enoxacin gluconate crude product, first stir the enoxacin gluconate solution obtained in step A) for 300min again, then filter, concentrate the filtrate under reduced pressure, the reduced pressure is -0.95MPa, concentrate the concentrate To 1 / 2 of the volume of enoxacin gluconate solution, the concentration temperature is 70°C, then cooling and crystallization, the temperature of cooling and crystallization is 8°C, suction filtration and drying, the drying temper...

Embodiment 3

[0030] A) To prepare enoxacin gluconate solution, add gluconic acid to the purified water equipped with a stirring device and meet the standards of the Chinese Pharmacopoeia to dissolve the gluconic acid in the purified water, add enoxacin to stir the reaction, and statically Put 10h, obtain enoxacin gluconate solution, in this step, the weight ratio of gluconic acid, purified water and enoxacin is 1.5: 5: 2, the temperature of described stirring reaction is 30 ℃, the reaction time 330min;

[0031] B) To prepare the enoxacin gluconate crude product, first stir the enoxacin gluconate solution obtained in step A) for 200min again, then filter, concentrate the filtrate under reduced pressure, the reduced pressure is -0.9MPa, and concentrate the concentrate To 3 / 4 of the volume of enoxacin gluconate solution, the concentration temperature is 80°C, then cooling and crystallization, the temperature of cooling and crystallization is 4°C, suction filtration and drying, the drying ...

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Abstract

The invention provides a preparation method of enoxacin gluconate, belonging to the technical field of preparation of a quinolones antibacterial agent. The preparation method comprises the following steps of: dissolving gluconic acid in pure water in a reaction container with a stirring device; adding enoxacin to stir and react; standing so as to obtain an enoxacin gluconate solution; stirring the enoxacin gluconate solution again and then filtering; decompressing and concentrating a filtrate; cooling, crystallizing, leaching and drying, so as to obtain an enoxacin gluconate crude product; dissolving the enoxacin gluconate crude product in an ethanol solution; adding a decolorant to stir, decolorate and filter; cooling the filtrate with water; leaching after separating a crystal; washing a filter cake with absolute ethyl alcohol; and carrying out vacuum drying so as to obtain the fined enoxacin gluconate. The preparation method provided by the invention has the advantages as follows: the gluconic acid is dissolved in the pure water to stir and react at constant temperature, so that not only can the yield and the quality be obviously improved, but also the security in a preparation process is beneficial to being ensured, and the preparation cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of quinolone antibacterial drugs, in particular to a preparation method of enoxacin gluconate. Background technique [0002] Enoxacin (Enoxacin, ENX) is a third-generation quinolone drug (also known as a compound). It has been widely used in clinic as an oral preparation because of its broad antibacterial spectrum, good curative effect and small side effects. Both have good curative effect, and have attracted the attention of the medical circles all over the world. It is generally believed that its mechanism of action is that the drug binds to DNA helicase, and then inhibits the activity of the enzyme to play a role. Studies such as Shen have proved (Brumfitt W, Hamilton Miller JM, Shen, Enoxacin relieves symptoms of recurrent urinary infections more rapidly than cefuroxime axetil. Antimicrob Agents Chemother, 1993, 37 (7): 1558-1559), fluoroquinolones directly interact with DNA Combine, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04C07C59/105C07C51/41C07C51/42
Inventor 王多平姚宇
Owner JIANGSU HI STONE PHARMA
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