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Method for preparing 2,2'-dithiodibenzothiazole from waste residues generated during process of AE-active ester production

A technology of dithiodibenzothiazole and active ester, which is applied in the field of preparation of 2,2'-dithiodibenzothiazole, can solve the problems of complex operation, cumbersome recovery steps, unsuitability for large-scale production and application, and achieve The effect of high purity, fast reaction rate and low production cost

Active Publication Date: 2016-03-23
河北合佳医药科技集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many methods for recovering DM from AE-active ester production waste residues that have been disclosed at present, but most of the methods have cumbersome recovery steps and complicated operations, which are not suitable for large-scale production applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] This example relates to a method for preparing 2,2'-dithiodibenzothiazole from AE-active ester production waste residue. The used AE-active ester production waste residue has an M content of about 30%, and other substances contained include aminothioxamic acid, triethyl phosphate, AE-active ester, and the like.

Embodiment 11

[0016] The preparation of 2,2'-dithiodibenzothiazole from AE-active ester production waste residue specifically includes the following steps:

[0017] a. Dissolve 500kg of AE-activated ester production waste residue in 1000L of methanol, add 0.25kg of catalyst tetrabutylammonium bromide, then heat the reaction system to 40°C, then feed 20kg of ozone at 9.3 cubic meters per hour, at 90 rpm / minute stirring speed reaction 1h;.

[0018] b. After the reaction in step a is completed, stop feeding ozone and continue stirring. After keeping the system materials warm at 40°C for 1 hour, pass cold brine to cool down to 10°C, and pass the cooled system materials through a centrifuge at 900 rpm. Filter to collect the solid, and finally dry the solid in a double-cone vacuum dryer with a vacuum degree of 0.09-0.095Mpa and a temperature of 80-90°C for 4-5 hours to obtain 126kg of the product 2,2'-dithiodibenzothiazole , the reaction yield reached 96.5%.

[0019] The obtained product 2,2'...

Embodiment 12

[0021] The preparation of 2,2'-dithiodibenzothiazole from AE-active ester production waste residue specifically includes the following steps:

[0022] a. Dissolve 1000kg of AE-activated ester production waste residue in 2100L of methanol, add 0.6kg of catalyst tetrabutylammonium bromide, then heat the reaction system to 42°C, then feed 45kg of ozone at 9.5 cubic / hour, at 90 rpm Reaction 1h under the stirring speed of / minute;

[0023] b. After the reaction in step a is completed, stop feeding ozone and continue stirring. After keeping the system materials warm at 42°C for 1.5 hours, pass cold brine to cool down to 8°C, and pass the cooled system materials through a centrifuge at 900 rpm. Filter to collect the solid, and finally dry the solid in a double-cone vacuum dryer with a vacuum degree of 0.09-0.095Mpa and a temperature of 80-90°C for 4-5 hours to obtain the product 2,2'-dithiodibenzothiazole 254kg , the reaction yield reached 97.2%.

[0024] The obtained product 2,2'...

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Abstract

The invention relates to a method for preparing 2,2'-dithiodibenzothiazole from waste residues generated during the process of AE-active ester production. The method comprises the following steps: dissolving waste residues generated during the process of AE-active ester production into methanol, adding a catalyst (tetrabutyl ammonium bromide), introducing ozone into the reactions system at a temperature of 40 to 45 DEG C, carrying out reactions for 1 to 1.5 hours under stirring, after the reactions (a), stopping introducing ozone, keeping on stirring, maintaining the reaction temperature for 1 to 1.5 hours, then cooling to a temperature of 5 to 10 DEG C, filtering, and drying the reaction product in vacuum to obtain 2,2'-dithiodibenzothiazole. The provided method can high efficiently recover M from the waste residues generated during the process of AE-active ester production so as to produce high purity DM; moreover, the provided method has the advantages of simple technology, mild conditions, safety, and easiness in controlling, the used solvent is easy to recover and generates little pollution, the production cost is low, and the preparation method is suitable for large scale production.

Description

technical field [0001] The invention relates to a method for recycling production waste residue in the pharmaceutical field, in particular to a method for preparing 2,2'-dithiodibenzothiazole from AE-active ester production waste residue. Background technique [0002] AE-active ester, chemical name 2-methoxyimino-2-(2-amino-4-thiazolyl)-(z)-benzothiazolyl thioacetate, is the third generation cephalosporin antibiotic cephalosporin An important intermediate of trixone and cefotaxime, widely used. AE-active ester is synthesized from aminothiaxamic acid and 2,2'-dithiodibenzothiazole (DM for short). During the synthesis reaction of AE-active ester, the raw material DM will be decomposed into two 2-thiobenzothiazoles (referred to as M), wherein one M is synthesized into AE-active ester with aminothiaxamic acid, and the other M remains in the AE-active ester production waste residue, which will cause great pollution to the environment and increase production costs. Therefore, it ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
CPCC07D277/78
Inventor 刘振强董永利王荣霞臧传梅
Owner 河北合佳医药科技集团股份有限公司
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