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Novel process for producing medical intermediate DM (dibenzothiazyl disulfide)

A technology for intermediates and new processes, applied in the field of new processes for the production of pharmaceutical intermediates DM, can solve the problems of large-scale industrial production of CsF-Celite, adverse effects of the surrounding environment, and low impurity content, so as to shorten the reaction time and improve the quality. Ideal, high safety factor effect

Active Publication Date: 2013-01-09
温州市嘉力新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to obtain high-quality DM with low impurity content, high melting point, and short melting range, a method for preparing DM by oxygen oxidation in the presence of CsF-Celite has been reported abroad; although the quality of DM obtained by this method is relatively good, it can reach The requirements for manufacturing drugs, but only limited to the laboratory level, CsF-Celite is difficult to use in large-scale industrial production
Lanzhou Petrochemical Research Institute has developed a method of refining industrial DM with benzene solvents to produce high-purity medicinal DM. The melting point of the obtained DM can reach 181°C and the content exceeds 98%, which meets the requirements for the manufacture of AE active esters; however, benzene solvents are used , will have adverse effects on both personnel and the surrounding environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Put 500 kilograms of 2-mercaptobenzothiazole (M) into a reaction kettle filled with 2.8 cubic meters of isopropanol aqueous solution, stir well for 1 hour, and add 333 milliliters of triethylbenzyl ammonium chloride while stirring , and then add dropwise a mixture of isopropanol and 27.5% hydrogen peroxide at a rate of 280 liters per hour, wherein hydrogen peroxide and isopropanol are mixed at a ratio of 1:1, and the reaction temperature is controlled not to exceed 50°C during the dropping process. 450 liters of mixed solution; after adding the mixed solution A dropwise, react for another 30 minutes, and measure it with the cobalt oleic acid method. finished product. The measured data of DM products are shown in Table 1.

Embodiment 2

[0025] Put 525 kilograms of 2-mercaptobenzothiazole (M) into a reaction kettle filled with 1.75 cubic meters of isopropanol aqueous solution, stir thoroughly for half an hour, and add 375 milliliters of triethylbenzyl ammonium chloride while stirring , and then add dropwise a mixture of isopropanol and 27.5% hydrogen peroxide at a rate of 300 liters per hour, wherein hydrogen peroxide and isopropanol are mixed at a ratio of 1:1, and the reaction temperature is controlled not to exceed 50°C during the dropping process. 656 liters of mixed solution; after adding the mixed solution A dropwise, react for another 60 minutes, and measure it with the cobalt oleic acid method. finished product. The measured data of DM products are shown in Table 1.

Embodiment 3

[0027] Put 525 kilograms of 2-mercaptobenzothiazole (M) into a reaction kettle filled with 4.0 cubic meters of isopropanol aqueous solution, stir thoroughly for half an hour, and add 393 milliliters of triethylbenzyl ammonium chloride while stirring , and then add dropwise a mixture of isopropanol and 27.5% hydrogen peroxide at a rate of 200 liters per hour, wherein hydrogen peroxide and isopropanol are mixed at a ratio of 1:1, and the reaction temperature is controlled not to exceed 50°C during the dropping process. 350 liters of mixed solution; after adding the mixed solution A dropwise, react for another 30 minutes, and measure it with the cobalt oleic acid method. finished product. The measured data of DM products are shown in Table 1.

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Abstract

The invention relates to a novel process for producing a medical intermediate DM (dibenzothiazyl disulfide). The process comprises the following step of: oxidizing 2-thiolbenzothiazole under the catalytic action of benzyltriethylammonium chloride serving as a catalyst at the temperature of lower than 50 DEG C by taking hydrogen peroxide as an oxidant and taking an isopropanol aqueous solution as a solvent. The benzyltriethylammonium chloride serving as the catalyst is adopted, so that the conversion rate of M is almost up to 100 percent, and the reaction rate is increased; isopropanol is selected as a reaction solvent, is recycled in a production process, is environmentally-friendly, and is low in toxicity; an obtained product has very ideal quality (the melting pint is more than or equal to 178.0 DEG C, and the content is more than or equal to 98.0 percent); all used raw materials are industrial grade products, are low in cost, are readily-available, and have good economic benefits; and in an entire reaction process, a normal pressure state is kept, the temperature does not surpass 50 DEG C, the safety coefficient is high, and the entire reaction process is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a new production process of pharmaceutical intermediate DM. Background technique [0002] For the organic synthetic chemical industry, the research and development of green and clean synthetic processes has important strategic significance. It can not only save resources and reduce environmental burdens, but also realize sustainable industrial production and create good economic and social benefits. There are several ways to realize green chemistry in organic synthesis: design of target molecules; use of non-toxic and non-hazardous raw materials; use of non-toxic and non-hazardous (low) solvents; Use non-toxic and non-hazardous catalysts; use more advanced equipment and milder reaction conditions. [0003] With the discovery of monocyclic β-lactam antibiotics, the research on the method of synthesizing β-lactams has been further promoted, and a variety of synthetic process route...

Claims

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Application Information

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IPC IPC(8): C07D277/78
Inventor 林立
Owner 温州市嘉力新材料有限公司
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