Production method of 1-methyl-5-mercapto-1,2,3,4-tetrazole

A production method and a technology for tetrazolium, which are applied in the field of chemical synthesis and preparation, can solve the problems of intractability, large recovery loss and low yield, achieve significant economic and social benefits, reduce production costs and environmental pollution, and reduce product yields. high rate effect

Active Publication Date: 2010-07-21
山东艾孚特科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] But this method has problems such as low yield, large amount of three wastes and difficult to handle, especially the large loss of ethanol in the recovery of synthetic solvents, and the low boiling point of chloroform in the recrystallization of chloroform. It has a great impact on the environment and does not meet the requirements of developing green chemistry and promoting clean production at home and abroad

Method used

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  • Production method of 1-methyl-5-mercapto-1,2,3,4-tetrazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 700L of deionized water into the reaction kettle, start stirring, add 300Kg of sodium azide, add 0.8kg of high-efficiency phase transfer catalyst tetrabutylammonium chloride, heat up to 80°C with steam, switch to circulating water to cool down, and start dripping molten 405kg of methyl isothiocyanate, control the rate of addition, and ensure that the temperature of the reaction system is around 80°C. After the dropwise addition is completed, the heat preservation reaction is carried out for 5 hours. After the heat preservation is completed, the reaction solution is transferred to the dehydration kettle, and concentrated under reduced pressure. , stop concentrating, pass circulating water to cool down to room temperature, switch to refrigerated brine and continue to cool down to -5°C, add hydrochloric acid dropwise, measure the pH value of the reaction solution, the Congo red test paper changes from red to blue as the end point, crystallize for 2 hours, and centrifuge ...

Embodiment 2

[0018] Add 700L of deionized water into the reactor, start stirring, add 300Kg of sodium azide, add 1kg of high-efficiency phase transfer catalyst 18-crown 6 ether, heat up to 70°C with steam, switch to circulating water to cool down, and start adding molten isosulfur Methyl cyanate 405kg, control the rate of addition, and ensure that the temperature of the reaction system is around 70°C. After the dropwise addition is completed, the temperature is kept for 8 hours. After the temperature is completed, the reaction solution is transferred to the dehydration kettle, and concentrated under reduced pressure. When the concentration is about half, stop the concentration After cooling down to room temperature with circulating water, switch to frozen brine and continue to cool down to -5°C, add hydrochloric acid dropwise, measure the pH value of the reaction solution, the Congo red test paper changes from red to blue as the end point, keep crystallization at -5°C for 2 hours, leave 500...

Embodiment 3

[0021] Add 1200L of deionized water into the reactor, start stirring, add 300Kg of sodium azide, add 18kg of high-efficiency phase transfer catalyst trioctylmethyl ammonium chloride, heat up to 80°C with steam, switch to circulating water to cool down, and start dropping Molten methyl isothiocyanate 405kg, control the rate of addition, to ensure that the temperature of the reaction system is around 80 ° C, after the dropwise addition is completed, the heat preservation reaction is 5 hours, after the heat preservation is completed, the reaction solution is transferred to the dehydration kettle, and concentrated under reduced pressure. , stop the concentration, pass circulating water to cool down to room temperature, switch to frozen brine and continue to cool down to -5°C, add hydrochloric acid dropwise, measure the pH value of the reaction solution, the Congo red test paper changes from red to blue as the end point, keep at -5°C After crystallization for 2 hours, 560Kg of crude...

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Abstract

The invention discloses a production method of 1-methyl-5-mercapto-1,2,3,4-tetrazole, which comprises the following steps of: dropwise adding methyl isorhodanate into a system of sodium azide, a high-efficiency phase transfer catalyst and deionized water, reacting at 50-100 DEG C for 1-10 hours, concentrating, cooling, acidizing, crystallizing, and centrifuging to obtain rough 1-methyl-5-mercapto-1,2,3,4-tetrazole; after carrying out alkali dissolving, active carbon decoloring, filtering and impurity removing, acidizing, crystallizing and centrifuging on the rough product, adding hydrogen peroxide and water, recrystallizing, centrifuging and drying to obtain a finished product. The method has simple operation, high product yield, no use of organic solvent with reaction processes and product fining process which are all carried out under an aqueous solvent environment, thereby greatly reducing the production cost and the environmental pollution, meeting requirements of clean production and having remarkable economical and social benefits.

Description

technical field [0001] The invention relates to a production method of 1-methyl-5-mercapto-1,2,3,4-tetrazolium, belonging to the field of chemical synthesis preparation. Background technique [0002] 1-Methyl-5-mercapto-1,2,3,4-tetrazolium (referred to as MMT), English name: 1-Methyl-5-mercapto-1,2,3,4- Tetrazole, CAS number: [13183-79-4], molecular formula: C 2 h 4 N 4 S, molecular weight 116.15, white crystal, soluble in water, chloroform, ether, etc., melting point: 125.0-127.0°C. It is an important intermediate of various products of the third, fourth, and fifth generations of cephalosporin antibiotics, and is mainly used in the synthesis of cefoperazone, cefamandole, cefmenoxime, cefpiramide, cefuroxime, cefazin, cefavitrix, More than 10 kinds of cephalosporin antibiotic pharmaceutical products, such as cephalosporin aminothiauron, cephalosporin, cephalosporin sulfadiazine, cephalosporin benzopyrazole, and cephalosporin nalidixin. [0003] At present, the method of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/04
Inventor 冯维春孟宪兴王灏胡波刘丽秀邢伶常丽霞
Owner 山东艾孚特科技有限公司
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