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Method for preparing medicine grade DM with technical grade DM

A pharmaceutical-grade and industrial-grade technology, applied in the field of DM preparation, can solve problems such as poor process safety, high equipment requirements, and pollute the environment, and achieve the effects of low equipment requirements, no pollution to the environment, and avoidance of toxic substances.

Inactive Publication Date: 2010-07-28
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 2. Poor process safety
[0005] 3. High equipment requirements and large investment
[0006] 4. Pollution of the environment

Method used

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  • Method for preparing medicine grade DM with technical grade DM
  • Method for preparing medicine grade DM with technical grade DM

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The method for preparing pharmaceutical grade DM with industrial grade DM of the present invention comprises the following steps:

[0023] (1) Dissolution: use industrial grade DM as raw material, tetrachlorethylene as solvent, dissolve in a dissolution kettle at 100-150°C, and the weight ratio of industrial grade DM to tetrachlorethylene is 1:10;

[0024] (2) Adsorption: adding activated carbon to the above-mentioned solution, the weight of the activated carbon accounts for 0.1% by weight of the above-mentioned solution, and stirs for 2 hours;

[0025] (3) Filtration: the above solution is filtered to separate activated carbon;

[0026] (4) Crystallization: Cool the above solution to 0°C, and DM crystallizes out;

[0027] (5) Filtration: Filter the above solution to separate pharmaceutical grade DM;

[0028] (6) Drying: In a vacuum dryer, dry the separated pharmaceutical grade DM to obtain a finished product. The drying temperature is 100-110°C, the vacuum degree is ...

Embodiment 2

[0031] The method for preparing pharmaceutical-grade DM with industrial-grade DM of the present invention is special in that it comprises the following steps:

[0032] (1) Dissolution: use industrial grade DM as raw material, tetrachlorethylene as solvent, dissolve in a dissolution kettle at 100-150°C, and the weight ratio of industrial grade DM to tetrachlorethylene is 1:35;

[0033] (2) Adsorption: add activated carbon to the above solution, the weight of activated carbon accounts for 5% by weight of the above solution, and stir for 1 hour;

[0034] (3) Filtration: the above solution is filtered to separate activated carbon;

[0035] (4) Crystallization: Cool the above solution to 50°C, and DM crystallizes out;

[0036] (5) Filtration: Filter the above solution to separate pharmaceutical grade DM;

[0037] (6) Drying: In a vacuum dryer, dry the separated pharmaceutical grade DM to obtain a finished product. The drying temperature is 100-110°C, the vacuum degree is 0.05-0.0...

Embodiment 3

[0039] The method for preparing pharmaceutical-grade DM with industrial-grade DM of the present invention is special in that it comprises the following steps:

[0040] (1) Dissolution: use industrial grade DM as raw material, tetrachlorethylene as solvent, dissolve in a dissolution kettle at 100-150°C, and the weight ratio of industrial grade DM to tetrachlorethylene is 1:22;

[0041] (2) Adsorption: adding activated carbon to the above solution, the weight of the activated carbon accounts for 2.5% by weight of the above solution, and stirs for 1.5 hours;

[0042] (3) Filtration: the above solution is filtered to separate activated carbon;

[0043] (4) Crystallization: Cool the above solution to 25°C, and DM crystallizes out;

[0044] (5) Filtration: Filter the above solution to separate pharmaceutical grade DM;

[0045] (6) Drying: In a vacuum dryer, dry the separated pharmaceutical grade DM to obtain a finished product, the drying temperature is 100-110°C, the vacuum degre...

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PUM

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Abstract

The invention provides a method for preparing a pharmaceutical grade DM by an industrial grade DM, comprising the following steps of: (1) dissolution; (2) adsorption; (3) filtration; (4) crystallization; (5) filtration; and (6) drying. The method has the advantages of non toxic and side-effect to human body by using perchlorethylene to substitute toluene as a solvent, safety and reliability, avoiding the defect of discharge of poisonous substances to the air, non environmental pollution, good process safety, low equipment requirements and low investment.

Description

(1) Technical field [0001] The invention belongs to a method for preparing DM, in particular to a method for preparing medical-grade DM with industrial-grade DM. (2) Background technology [0002] Pharmaceutical grade DM (dibenzothiazole disulfide) is the raw material for the production of pharmaceutical intermediates—AE active ester products, and AE active ester products are raw materials for the production of cephalosporin antibiotics. In recent years, the rapid development of cephalosporin antibiotic products has stimulated the development of pharmaceutical grade DM. At present, the process of producing pharmaceutical-grade DM in my country is to use industrial-grade DM (dibenzothiazole disulfide) as raw material and toluene as solvent to obtain pharmaceutical-grade DM through recrystallization. Its process is: melting adsorption filter recrystallization filter dry. Toluene was distilled and reused. The disadvantages of this process are: [0003] 1. Use toxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/78
Inventor 徐承秋金福盛单世超刘经福吕桂中周福鹏刘园园
Owner SHANDONG SUNSINE CHEM