Post processing method for preparing levo-ofloxacin

A levofloxacin and crude product technology, which is applied in the post-treatment field of levofloxacin preparation, can solve the problems related to the increase of impurity content, achieve the effects of increasing yield, avoiding environmental problems, and reducing the unit consumption of solvents

Inactive Publication Date: 2005-10-26
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Also available image 3 The process shown in the preparation of levofloxacin finished product, bu

Method used

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  • Post processing method for preparing levo-ofloxacin
  • Post processing method for preparing levo-ofloxacin
  • Post processing method for preparing levo-ofloxacin

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Put 100 grams of levofluorocarboxylic acid into the reaction flask, then add 400 milliliters of dimethyl sulfoxide and 100 milliliters of N-methylpiperazine, heat and control the inner temperature of 85 ° C for 5 hours; after TLC analysis is qualified, recover N -Methylpiperazine and dimethyl sulfoxide, keep the internal temperature below 100°C. Add 400 milliliters of water to the obtained product to adjust the pH=6.0 to 6.5, add 1.5 grams of activated carbon after dissolving and keep stirring for 30 minutes to carry out acid-dissolving and refining. Then filter, heat to 65-75°C, adjust the pH to 9.5-10.0 with sodium hydroxide solution, add 1.5 grams of activated carbon and keep stirring for 30 minutes to carry out alkali-dissolving refinement, and then filter. Add an appropriate amount of hydrochloric acid to adjust the pH to 7.0-8.0 while stirring, add 200 ml of chloroform for extraction, repeat the chloroform extraction for 6-10 times, combine the extracts, recover t...

Embodiment 2

[0030] 100 grams of levofloxacin was fed, and the levofloxacin crude product was prepared as described in Example 1, with a wet weight of 163 grams.

[0031] Add 600 ml of absolute ethanol to the levofloxacin wet product, heat up in a water bath, and after the dissolution is complete, add a small amount of EDTA and activated carbon, keep warm at 60-75°C for 30 minutes, filter, add about 30 ml of 15% sulfuric acid to the filtrate, cool and crystallize , filtered to obtain levofloxacin sulfate, with a wet weight of 185 grams.

[0032] Add 550 ml of absolute ethanol and 25 ml of 5% ammonia water to the levofloxacin hydrochloride sulfate wet product, heat up in a water bath, and after the dissolution is complete, add a small amount of EDTA and activated carbon, keep warm at 60-75°C for 30 minutes, filter, and the filtrate is cooled and crystallized , filter the obtained crystals and dry under reduced pressure with a water pump for 2.0 to 3.0 hours at a temperature of 50 to 55° C. ...

Embodiment 3

[0034] 100 grams of levofloxacin was fed, and the levofloxacin crude product was prepared as described in Example 1, with a wet weight of 167 grams.

[0035] Add 600 ml of absolute ethanol to the wet product of levofloxacin, heat up in a water bath, and after the dissolution is complete, add a small amount of EDTA and activated carbon, keep warm at 60-75°C for 30 minutes, filter, add about 30 ml of concentrated hydrochloric acid to the filtrate, cool and crystallize, Filter to obtain levofloxacin hydrochloride, wet weight 170 grams.

[0036] Add 550 ml of absolute ethanol to the wet product of levofloxacin hydrochloride, adjust the pH to 7.5-8.0 with saturated sodium bicarbonate solution, heat up in a water bath, and after the dissolution is complete, add a small amount of EDTA and activated carbon, and keep warm at 60-75°C for 30 minutes. Filtrate, cool the filtrate to crystallize, and dry the obtained crystals with a water pump under reduced pressure for 2.0 to 3.0 hours at ...

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Abstract

The present invention provides an after-treatment method for preparation of levofloxacin. Said method is characterized by that after reaction with methylpipie it can directly recover solvent, and adopts the method of firstly salt-forming and then using alkali to make neutralization so as to effectively obtain levofloxacin with high purity.

Description

Technical field: [0001] The invention relates to medicinal chemistry, in particular to a post-treatment method for preparing levofloxacin. Background technique: [0002] Fluoroquinolones have achieved great success in clinical anti-infection treatment due to their high-efficiency, broad-spectrum, and low-toxicity antibacterial properties. Ofloxacin and Levofloxacin developed by Japan's Daiichi Pharmaceutical Company are among them Excellent variety. Levofloxacin is the S enantiomer of racemic ofloxacin, and the antibacterial activity of ofloxacin is mainly attributed to the S enantiomer. [0003] Levofloxacin is a chiral fluorinated quinolone structure, its chemical name is S-(-)9-fluoro-3-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-2 , 3-Dihydro-7H-pyrido-[1,2,3,-de][1,4]benzoxazine-6-carboxylic acid hemihydrate (CAS Registry No. 100986-85-4). The chemical structure of levofloxacin is shown in formula 1. [0004] [0005] Formula 1 [0006] There are ma...

Claims

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Application Information

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IPC IPC(8): C07D498/06
Inventor 吴国锋杨朱红梁赛红徐国兴陈兴江
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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