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Method for producing high-content pharmaceutical grade MBT

A production method and a pharmaceutical-grade technology are applied in the field of MBT refining of pharmaceutical intermediates, which can solve the problem of low MBT purity and achieve the effects of high melting point, short melting range and easy industrialization.

Active Publication Date: 2009-12-02
内蒙古科迈化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can only remove a small amount of resin and impurities, and the purity of the refined MBT is not high, and because MBT is in contact with the toxic solvent toluene, there is a danger of bringing toxic substances into downstream products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Condensation reaction of aniline with carbon disulfide and sulfur at 270-280°C and pressure of 9-10Mpa produces crude MBT with a mass percentage of 75%, and the remaining impurities include: resin 20% and intermediate product 5%. 223 grams of 75% by mass percentage of crude MBT is dissolved in 4000 grams of 1% sodium hydroxide aqueous solution at 20°C and a rotating speed of 200 rpm at 20°C, and filtered after completely dissolving. , rotating speed is under the condition of 200 rev / mins, in the filtrate, drip the mixed solution that is 10% hydrogen peroxide and the sulfuric acid of 20% by mass percentage in the filtrate, when the solution color turns yellow-green, stop reaction, after filtering, use The mass percent is 5% sulfuric acid solution to neutralize the filtrate, and when the Ph value is 7, obtain 167.8 grams of high-content pharmaceutical grade MBT after filtering, washing and drying. The 2-mercaptobenzothiazole has a mass percentage of 99.5% and a melting po...

example 2

[0010] The crude MBT used in this example is the same as that in Example 1. 223 grams of crude MBT with a mass percentage of 75% is dissolved in 3333 grams of 3% hydrogen at 45° C. and a rotating speed of 750 rpm. In the sodium oxide aqueous solution, filter after being completely dissolved, and at 45°C and a rotating speed of 750 rpm, add dropwise a mixed solution of 25% hydrogen peroxide and 50% sulfuric acid in the filtrate, when When the color of the solution turns yellow-green, the reaction is stopped, and after filtration, 10% sulfuric acid solution is used to neutralize the filtrate. When the Ph value is 7, filter, wash, and dry to obtain 167.6 grams of high-content pharmaceutical grade MBT. The 2-mercaptobenzothiazole has a mass percentage of 99.6% and a melting point of 180.9°C.

example 3

[0012] The process for synthesizing crude MBT used in this example is the same as that in Example 1. 223 grams of 75% by mass percentage of crude MBT is dissolved in 2667 grams of 6% sodium hydroxide aqueous solution at 70°C and a rotating speed of 1200 rpm at 70°C, and filtered after completely dissolving. , rotating speed is under the condition of 1200 rev / mins, in the filtrate, dropwise add the mixed solution of the hydrogen peroxide of 40% mass percent and the sulfuric acid of 70% by mass percent, when the solution color turns yellow-green, stop reaction, after filtering, use The mass percent is 15% sulfuric acid solution to neutralize the filtrate, and when the Ph value is 7, obtain 167.2 grams of high-content pharmaceutical grade MBT after filtering, washing and drying. The 2-mercaptobenzothiazole has a mass percentage of 99.9% and a melting point of 181.6°C.

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Abstract

The invention discloses a method for producing high-content pharmaceutical grade MBT. The method comprises the following processes: dissolving 50 to 80 mass percent crude MBT into 1 to 6 mass percent sodium hydroxide water solution according to the molar ratio of the crude MBT to sodium hydroxide of 1:1-4 at the temperature of between 20 and 70 DEG C under the rotating speed of 200 to 1,200 revolutions per minute, filtering the mixture after the crude MBT is fully dissolved, dropping mixed solution of 10 to 40 mass percent hydrogen peroxide and 20 to 70 mass percent sulfuric acid into the filtrate at the temperature of between 20 and 70 DEG C under the rotating speed of 200 to 1,200 revolutions per minute, stopping the reaction after the color of the solution becomes yellow green, using 5 to 15 mass percent sulfuric acid solution to neutralize the filtrate after filtration, and filtering, washing and drying a product when the pH value is 7 to obtain the high-content pharmaceutical grade MBT. The method has the advantages that the method has simple process and is easy for industrialization, the purity of the obtained refined MBT reaches more than 99.5 percent, and the MBT has high melting point and short melting range.

Description

technical field [0001] The invention relates to a production method of high-content pharmaceutical grade 2-mercaptobenzothiazole (MBT), which belongs to the technical field of refining pharmaceutical intermediate MBT. Background technique [0002] With the development of society, the research and production of pharmaceutical intermediates are getting more and more attention. The pharmaceutical intermediate MBT is an essential raw material for the preparation of cephalosporin anti-inflammatory drugs, but because it is used in the pharmaceutical field, the content of MBT is extremely high, so MBT must be refined before it can be used. Usually, the impurities in the pharmaceutical intermediates are mainly resins and intermediate products (such as benzothiazole), and the existence of impurities makes the product quality not high. Literature (Fine Chemical Raw Materials and Intermediates, 2003, 1:40) reported the method of refining MBT. The crude MBT melt is dissolved in a mixt...

Claims

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Application Information

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IPC IPC(8): C07D277/72
Inventor 朱军李树东路树元王树华王树领王树恒
Owner 内蒙古科迈化工有限公司
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