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Comprehensive recycling method of 2-mercaptobenzothiazole, triethylamine, and dichloromethane in ceftriaxone sodium dichloromethane mother liquid

A technology of mercaptobenzothiazole and ceftriaxone sodium, which is applied in the field of comprehensive recovery of 2-mercaptobenzothiazole, triethylamine and dichloromethane, can solve the problems of M purity reduction, harm, and environmental pollution, and achieve reduction The amount of alkali used, the effect of good performance and good practical prospects

Active Publication Date: 2018-12-21
SHANXI WEIQIDA PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following defects in this method: 1. ceftriaxone sodium mother liquor will have a certain amount of unknown impurity decomposed to produce after high-temperature distillation, and it is easy to separate out together with M in the crystallization process, so that the purity of M is reduced; 2. after the separation of M is not involved in the method The treatment method of the residual liquid, if the undistilled organic solvent is directly discharged, it will pollute the environment and cause great harm
[0007] As mentioned above, dichloromethane, M, and triethylamine are contained in the dichloromethane mother liquor produced in the production process of ceftriaxone sodium, but none of the above methods involves the recovery of triethylamine

Method used

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  • Comprehensive recycling method of 2-mercaptobenzothiazole, triethylamine, and dichloromethane in ceftriaxone sodium dichloromethane mother liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) reclaim 2-mercaptobenzothiazole

[0035] Get ceftriaxone sodium dichloromethane mother liquor 3L (M content: 4wt%, triethylamine content: 3wt%, dichloromethane content: 91.5wt%, impurity 1.5wt%), add 3L water, with 30wt% sodium hydroxide The pH value of the solution is adjusted to 12, and the temperature is controlled at 10-15°C during the adjustment process, vigorously stirred for 1 hour, and left to separate phases to obtain an organic phase 1 and an aqueous phase 1; The value is adjusted to 6, the temperature is controlled at 15°C-20°C during this process, and a large amount of khaki solid is precipitated, then filtered, washed with water, and dried to obtain 146.1g of 2-mercaptobenzothiazole, with a content of 98.56% (as determined by liquid chromatography, quantitative analysis) , the recovery rate was 92.3%. At the same time, the filtered filtrate (ie waste water 1) was collected.

[0036] (2) reclaim triethylamine

[0037] Add 3L of the filtrate (i.e. wast...

Embodiment 2

[0042] (1) reclaim 2-mercaptobenzothiazole

[0043] Get ceftriaxone sodium dichloromethane mother liquor 3L (M content: 4wt%, triethylamine content: 3wt%, dichloromethane content: 91.5wt%, impurity 1.5wt%), add 3L embodiment 1 step (2) recovery Wastewater 2 produced by triethylamine, the pH value is adjusted to 13 with 30wt% sodium hydroxide solution, the temperature is controlled at 15-20°C during the adjustment process, vigorously stirred for 2 hours, and the phases are separated to obtain the organic phase 1 and the water phase 1. Adjust the pH value of the water phase 1 to 9 with 92.5wt% sulfuric acid. During this process, the temperature is controlled at 5°C-10°C, and a large amount of khaki solid is precipitated, then filtered, washed with water, and dried to obtain 143.7g of 2-mercaptobenzothiazole , content 98.21% (as determined by liquid chromatography, quantitative analysis), recovery 90.5%. Collect the filtered filtrate (i.e., waste water 1) at the same time.

[0...

Embodiment 3

[0050] (1) reclaim 2-mercaptobenzothiazole

[0051] Get ceftriaxone sodium dichloromethane mother liquor 3L (M content: 4wt%, triethylamine content: 3wt%, dichloromethane content: 91.5wt%, impurity 1.5wt%), add step (2) in 3L embodiment 2 Recover the waste water 2 produced by triethylamine, adjust the pH value to 13 with 30wt% sodium hydroxide solution, control the temperature at 15-20°C during the adjustment process, stir vigorously for 1 hour, and stand to separate the phases to obtain the organic phase 1 and water Phase 1; the pH value of the aqueous phase 1 was adjusted to 7 with 50wt% sulfuric acid, and the temperature was controlled at 5°C-10°C during this process, and a large amount of khaki solid was precipitated, then filtered, washed with water, and dried to obtain 144.8g of 2-mercaptobenzothiazole , content 98.28% (determination by liquid chromatography, quantitative analysis), recovery rate 91.2%. At the same time, the filtered filtrate was collected.

[0052] (2...

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Abstract

The invention discloses a comprehensive recycling method of 2-mercaptobenzothiazole, triethylamine, and dichloromethane in a ceftriaxone sodium dichloromethane mother liquid. The method provided by the invention comprises: (1) recycling 2-mercaptobenzothiazole, (2) recysling triethylamine, and (3) recycling dichloromethane. The invention relates to a complete set of comprehensive recycling schemeof the ceftriaxone sodium dichloromethane mother liquid. According to the invention, the method provided by the invention has the advantages of simple operation, high yield, low cost, little pollutionand the like; the comprehensive recycling of 2-mercaptobenzothiazole, triethylamine, and dichloromethane can be implemented; the recycling of organic matter is maximized, and organic pollution environment is reduced; waste water generated from a recycling process is applied for reducing the dosage of acid and alkali in an extraction process, and meanwhile, the discharge of waste water is also controlled. The method provided by the invention has a good practical prospect.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and relates to a comprehensive recovery method for 2-mercaptobenzothiazole (abbreviated as M), triethylamine and methylene chloride in ceftriaxone sodium dichloromethane mother liquor. Background technique [0002] Ceftriaxone sodium is a third-generation broad-spectrum, high-efficiency, long-acting, and low-toxic cephalosporin, which is widely used in clinical practice. The main method of producing ceftriaxone sodium at present is: use 7-ACA as the main raw material and triazine ring condensation to generate 7-ACT intermediate, 7-ACT and AE active ester are catalyzed by triethylamine under methanol-dichloromethane system The reaction generates ceftriaxone sodium, and the by-product M is produced simultaneously; after adding water and sodium acetate to the reaction solution for reaction, the layers are left to stand, and the water layer carries out the crystallization proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72C07C209/86C07C211/05C07C17/383C07C19/03
CPCC07C17/383C07C209/86C07D277/72C07C211/05C07C19/03
Inventor 李伟白延峰李树有张俊锋王雁
Owner SHANXI WEIQIDA PHARMA IND
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