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Recovering and applying method of triethylamine in acylation liquid for preparing levofloxacin 1

A technology of levofloxacin and triethylamine, which is applied in the field of recovery and application of triethylamine in levofloxacin acylation solution, can solve the problems of serious pollution, difficult handling of triethylamine, high production cost, etc., achieve good effect, high recovery rate, and reduce The effect of production costs

Active Publication Date: 2011-08-17
ZHEJIANG LANGHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The triethylamine in the waste water of this process is not easy to handle, causing serious pollution and resulting in higher production costs

Method used

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  • Recovering and applying method of triethylamine in acylation liquid for preparing levofloxacin 1

Examples

Experimental program
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Effect test

Embodiment 1

[0024] The above filter cake triethylamine hydrochloride was adjusted to pH 12 with 10% NaOH, heated to 25°C, and extracted three times with 210g toluene, and the extract was dehydrated with calcium oxide to obtain 234g dry triethylamine / toluene solution. Ethylamine content 12.5wt%, recovery rate 96.5%, the calculation method of recovery rate is the ratio of the amount of triethylamine in the amount of triethylamine in 234g triethylamine / toluene solution and the amount of triethylamine in 41.3g filter cake triethylamine hydrochloride .

Embodiment 2

[0026] The above filter cake triethylamine hydrochloride was adjusted to PH to 12 with 20% NaOH, heated to 25°C, and extracted three times with 300g toluene, and the extract was dehydrated by calcium oxide to obtain 326.1g of dry triethylamine / toluene solution. The content of triethylamine is 9.23wt%, and the recovery rate is 99.3%.

Embodiment 3

[0028] Use 30% NaOH to adjust the pH to 14 with the above filter cake triethylamine hydrochloride, heat it to 25°C, extract it three times with 300g toluene, and dehydrate the extract with calcium oxide to obtain 328g dry triethylamine / toluene solution. The content of ethylamine is 9.15wt%, and the recovery rate is 99%.

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Abstract

The invention relates to a recovering and applying method of triethylamine in an acylation liquid for preparing levofloxacin 1 by a 2,3,4,5-tetrachloro benzoyl chloride acxylation method, belonging to the technical field of fine chemicals. The method is realized by the following steps: 1) filtering the acylation liquid in the process of preparing the levofloxacin by using the 2,3,4,5-tetrachloro benzoyl chloride acxylation method, so as to separate out the triethylamine, wherein the filtrate is an acylated mother liquid, and a filter cake is triethylamine hydrochloride; and 2) adding liquid alkaline to regulate the filter cake triethylamine hydrochloride to alkalinity, so that the triethylamine hydrochloride is converted into the triethylamine hydrochloride to be separated out, extractingwith an organic solvent, dehydrating and converting for synthesis. The triethylamine recovering method is simple to operate, rectification is not needed, and the recovery rate is high and reaches above 93% which is equivalent to the fact that about 35 kg of triethylamine is just added in production of 1 ton of levofloxacin 1, and for expensive triethylamine, production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a recovery method for triethylamine in levofloxacin acylation solution produced by acylation of 2,3,4,5-tetrabenzoyl chloride. Background technique [0002] Levofloxacin (Levofloxacin 1) chemical name: (S)-(-)-9-fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-7- Oxo-7H-pyridinebenzo[1,2,3-de]-[1,4]benzoxazine-6-carboxylic acid hemihydrate is the first fourth fluoroquinolone approved for production in my country Antibacterial drugs, which belong to the national essential drugs, have antibacterial effects, and their antibacterial strength is twice that of ofloxacin, and their toxicity is lower than that of ofloxacin. They are widely used clinically for respiratory tract infections, urinary tract infections, gynecological infections, liver tract infections Treatment of infections, eye infections, and intestinal infections. The structure of levofloxacin is a...

Claims

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Application Information

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IPC IPC(8): C07C209/74C07C211/05
Inventor 林邦平杜晓东蔡健
Owner ZHEJIANG LANGHUA PHARMA
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