Preparation method of amikacin

A technology of amikacin and kanamycin, which is applied in the field of medicine, can solve the problems of increasing solvent consumption costs, affecting personnel health, and using large solvents, so as to improve operability and safety, realize environmental friendliness, The effect of reducing solvent consumption

Active Publication Date: 2014-02-26
山东安信制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the poor activity of the commonly used catalysts, a large amount of flammable, explosive, and volatile solvents are required for the dissolution reaction. The use of solvents in the process is relatively large, and they are volatile, resulting in large losses, affecting the environment, and increasing costs.
Kanamycin sulfate has the disadvantages of low catalytic activity and slow catalytic silicification reaction, which usually takes about 28 hours and is not suitable for industrial production
Another commonly used catalyst, trimethylchlorosilane, has the following disadvantages, although its time is relatively short: (1) it is liquid at room temperature, and it is easy to absorb water in the air and undergo hydrolysis to release hydrogen chloride. On the one hand,...

Method used

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  • Preparation method of amikacin
  • Preparation method of amikacin
  • Preparation method of amikacin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 20g (41.3mmol) kanamycin A, add 66.6g (412.6mmol) hexamethyldisilazane, blow in nitrogen, add 0.2g micronized ammonium sulfate (d0.1=0.5um, d0.9≤ 5um), the temperature was controlled at 50°C, and no ammonia gas was released for 2 hours, evaporated to dryness with a high vacuum pump, and weighed 51.7g (because the product contained 0.2g ammonium sulfate, the calculated yield needs to be deducted, and the weight after deducting is 51.5g), Calculated according to full protection yield 97.5%. (No.: 1308001).

Embodiment 2

[0031] Take 20g (41.3mmol) kanamycin A, add 99.9g (619.0mmol) hexamethyldisilazane, blow in nitrogen, add 0.6g micronized ammonium sulfate (d0.1=0.3um, d0.9≤ 3um), the temperature was controlled at 70°C for reaction, no ammonia gas was released in 1 hour and 50 minutes, evaporated to dryness with a high vacuum pump, and weighed 52.3g (because the product contained 0.6g ammonium sulfate, the calculated yield needs to be deducted, and the weight after deducting is 51.7g ), the yield is 98.0% based on full protection. (No.: 1308002).

Embodiment 3

[0033] Take 20g (41.3mmol) kanamycin A, add 133.2g (825.3mmol) hexamethyldisilazane, blow in nitrogen, add 1.0g micronized ammonium sulfate (d0.1=0.1um, d0.9≤ 1um), the temperature was controlled at 80°C for 1 hour and 45 minutes, no ammonia gas was released, evaporated to dryness with a high vacuum pump, and weighed 53.0g (because the product contained 1.0g ammonium sulfate, the calculated yield needs to be deducted, and the weight after deducting is 52.0g) , The yield is 98.5% based on full protection. (No.: 1308003).

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Abstract

The invention discloses a preparation method of amikacin, belonging to the technical field of medicines. In a silylation reaction process, ammonium sulfate is micronized to remove a commonly-used solvent, hexamethyl disilazane is not only used as a reactant, but also used as a solvent, reaction time is shortened to about 2 hours, materials are easy to operate, and the preparation method is environment-friendly. Besides, in the silylation reaction process, a divalent metal organic weak acid salt is used as a complexing agent, so that the silylation reaction time can be shorted to about 1 hour; and meanwhile, selectivity of subsequent acylation reaction is improved, and yield of synthesizing the amikacin is improved.

Description

technical field [0001] The invention relates to a preparation method of amikacin, which belongs to the technical field of medicine. Background technique [0002] Amikacin sulfate is a semi-synthetic aminoglycoside antibiotic with a broad antibacterial spectrum and strong antibacterial ability against a variety of bacteria. Since its launch in the 1970s, amikacin sulfate has been widely used due to its definite curative effect, and has become the first-line anti-infective drug commonly used clinically in the world. In my country, Amikacin Sulfate has been included in the National Essential Drug List, and also included in the Class A drug in the "National Basic Medical Insurance and Work Injury Insurance Drug List". [0003] Amikacin, also known as amikacin. The most commonly used amikacin synthetic route is the silanization protection route (Jiang Zhongliang, Wang Yu. A new synthetic method of amikacin [J], Fine and Specialty Chemicals, 2004, 12 (10 ), 26-28). Specificall...

Claims

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Application Information

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IPC IPC(8): C07H15/234C07H1/00B01J35/10
Inventor 蔡成伟孙政军宿乾贞布彬彬王仕川樊长莹李保勇吴柯张兆珍董廷华
Owner 山东安信制药有限公司
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