Refining method of mercaptobenzothiazole disulfide
A technology of dibenzothiazole disulfide and refining method, which is applied in the direction of organic chemistry, can solve problems such as purity not higher than 99%, influence on recrystallization yield, batch yield disclosure, etc., to reduce production costs and achieve good social benefits and, the effect of increasing output
Inactive Publication Date: 2013-06-12
贾占军
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Problems solved by technology
However, there are three defects in this method. On the one hand, the solubility of toluene to DM is small, which leads to the disclosure of batch production.
On the other hand, due to the high international requirements for the quality of pharmaceutical grade DM, the initial melting point is required to be higher than 180°C, and the purity is not higher than 99%. The method of recrystallization with toluene cannot meet the requirements.
The third aspect, because the dissolution requires high temperature to dissolve, the solvent is volatile, and the solvent consumption is high
Although the purity reaches more than 99%, due to the non-selectivity of activated carbon adsorption, activated carbon not only adsorbs impurities in DM, but also adsorbs a certain amount of DM, resulting in a mixture of activated carbon and DM, which becomes waste and increases the consumption of DM. Crystallization yield
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Abstract
The invention relates to a refining method of mercaptobenzothiazole disulfide (DM). The refining method is characterized by comprising the following steps of: soakingindustrial grade DM with a solvent A, stirring for 10-30 hours at the temperature of 10-35 DEG C; stopping stirring, solid-liquid separating, washing the solid with a solvent B, and drying the solid, thereby obtaining the mercaptobenzothiazole disulfide. The refining method has the advantages of being low in material consumption, low in energy consumption, low in investment, high in output, safe, reliable and capable of greatly decreasing the production cost, thereby obtaining good social benefit.
Description
technical field [0001] The invention belongs to a method for refining pharmaceutical intermediates, in particular to a method for refining dibenzothiazole disulfide. Background technique Dibenzothiazole disulfide, referred to as DM in the industry, is mainly used in the rubber industry as an efficient accelerator for rubber vulcanization and crosslinking. The appearance is light yellow crystalline powder. Because this product has high thermal stability and stability against acid and alkali environment, it is used for high-grade rubber products. After the DM is purified, it becomes the pharmaceutical grade high-quality goods DM, which is the raw material drug 2-(2-amino-4-thiazolyl)-2-(methoxyimino)acetic acid thiobenzothiazolyl ester (AE- Active lipids) important intermediates and raw materials. The main impurity of industrial grade DM is mainly its monomer 2-mercaptobenzothiazole (accelerator M). Currently, the production and purification of pharmaceutical grade fine DM...
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IPC IPC(8): C07D277/78
Inventor 贾占军
Owner 贾占军