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Method using enzymolysis method to recycle kanamycin A from amikacin treating liquid

A kanamycin and amikacin technology, applied in the field of medicinal chemistry, can solve the problems of increased energy consumption for recovery, difficulty in operation, increased difficulty in production, and low recovery rate, and achieves easy industrial production, easy crystallization and separation, and reduced The effect of production costs

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Problems solved by technology

[0015] Patent CN109180752A discloses a method for recovering kanamycin A from amikacin synthetic liquid. This method is hydrolyzed at high temperature under alkaline conditions, the reaction time is very long, and the conditions are harsh, which increases the difficulty of large-scale production.
And still need to use macroporous cation exchange resin to purify, increase recovery energy consumption, operation difficulty, high cost, low recovery rate

Method used

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  • Method using enzymolysis method to recycle kanamycin A from amikacin treating liquid
  • Method using enzymolysis method to recycle kanamycin A from amikacin treating liquid
  • Method using enzymolysis method to recycle kanamycin A from amikacin treating liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: the preparation of amikacin synthetic liquid

[0038] Put 600m of acetonitrile into the silanization reaction bottle, put in 132g of kanamycin A (KMA), close the feeding port and start stirring for 10 minutes, then add 400mL of hexamethyldisilazane (HMDS), heat up to reflux, at 75~ Reflux reaction at 80°C for 7hr. After the reaction was completed, the temperature was lowered to below 35°C, left to stand, and the layers were separated naturally. The lower layer was separated and collected to obtain a silyl-protected product.

[0039] Add 1000mL of acetone to the silyl-protected product, start stirring, add 60g of γ-N-phthalimide-α-hydroxybutyric acid (PHBA), and then add 2.5g of catalyst 4-N,N-dimethyl Pyridine (DMAP), lower the temperature to -15°C to -10°C. Dissolve 60g of N,N-dicyclohexylcarbodiimide in 300mL of acetone, slowly add it to the above reactant at a controlled speed of 5mL / min, and control the temperature of the reactant at -15°C to -10°C;...

Embodiment 2

[0043] Embodiment 2: Purification treatment of amikacin synthetic liquid

[0044] 1510 mL of the amikacin synthetic solution obtained by the preparation method in Example 1 was purified by CD180 macroporous cation exchange resin, and eluted with ammonia water with a concentration of 0.5 mol / L, and the pure amikacin eluate and cardamom were collected respectively. The Namycin A eluate and the K29 eluate were concentrated to obtain 85.9 g of amikacin, 29.6 g of crude Kanamycin A, and 26.2 g of the K29 fraction, respectively.

Embodiment 3

[0045] Embodiment 3: the recovery preparation of kanamycin A

[0046] Add 26.2 g of the obtained K29 ​​component into a 1 L reaction vessel, add 130 ml of purified water, and stir to dissolve. Control the pH value of the feed solution to 7.8; add 0.26 g of immobilized enzyme CALB, and then stir and react at room temperature for 3 hours to generate a reaction solution containing kanamycin A; after the reaction is completed, filter and recover the immobilized enzyme CALB. Use 5M sulfuric acid in the filtrate to adjust the pH value of the reaction solution to 4.5, add 520ml of ethanol, cool down to 0-10°C, stir and crystallize for 3 hours; after crystallization, add concentrated ammonia water and stir to adjust the pH value to neutral, then filter and collect the solid 20.1g, the crude product of kanamycin A.

[0047]Combined with the 29.6g Kanamycin A crude product obtained in Combining Example 2, a total of 49.7g, with a purity of 96.0%. The above crude product can also be re...

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Abstract

The invention discloses a method using an enzymolysis method to recycle kanamycin A from amikacin treating liquid. The method includes: subjecting amikacin synthetic liquid to macroporous cation exchange resin purification, and collecting pure amikacin eluent, kanamycin A eluent and K29 eluent; allowing the K29 eluent and aminohydrolase to hydrolysis reaction at room temperature to obtain kanamycin A reaction liquid, filtering, adding acid into the filtrate to regulate pH to 4-5, cooling, adding an alcohol solvent, and performing heat preservation and crystallization to obtain crude kanamycin A, subjecting the kanamycin A eluent to reduced pressure distillation, and combining the distillation product with the crude kanamycin A to obtain all recycled kanamycin A. The method is mild in reaction condition, simple to operate, easy in crystallization, high in safety, capable of achieving raw material recycling and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a method for recovering kanamycin A from amikacin treatment liquid. Background technique [0002] Amikacin is a semi-synthetic aminoglycoside antibiotics, aminoglycoside antibiotics (Aminoglycosideantibiotics) have the structure of aminosugar and aminocycloalcohol, and are composed of aminosugar molecules and non-sugar part of the aglycone, used to treat a variety of Bacterial infections. Amikacin binds to the bacterial 30S subunit, blocks the expression and synthesis of bacterial proteins, and prevents bacterial elongation to achieve antibacterial effects. It has strong antibacterial ability against a variety of bacteria; its sulfate has become the first-line anti-infective drug commonly used clinically in the world. Since amikacin sulfate was launched on the market, it has been widely cited due to its definite curative effect and is mainly used for the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P19/48C07H15/234C07H1/06
CPCC12P19/485C07H15/234
Inventor 李法东周显峰陈中南杨庆坤李卓华郑长胜
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