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A kind of synthetic method of 1-(2-dimethylaminoethyl)-1h-5-mercapto-tetrazolium

A technology of -1H-5-, dimethylaminoethyl, which is applied in the field of synthesis of 1--1H-5-mercapto-tetrazolium, can solve the problem of less introduction of synthesis process, low yield of production process and complex equipment and other problems, to achieve the effects of environmental protection and easy waste salt treatment, avoiding biodegradation, and simple and easy post-treatment

Active Publication Date: 2022-04-08
河北凯力昂生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are few introductions to the synthesis process of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium, and there are problems such as high cost, low yield, and complicated equipment.
[0003] About the synthesis of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium at present mostly take N, N-dimethylethylenediamine and carbon disulfide as starting raw materials, then with dimethyl sulfate The ester undergoes a methylation process, and then reacts with sodium azide to form the final product. This process uses carbon disulfide and dimethyl sulfate. , a large amount of waste solids are produced, and the pressure on environmental protection is relatively high

Method used

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  • A kind of synthetic method of 1-(2-dimethylaminoethyl)-1h-5-mercapto-tetrazolium
  • A kind of synthetic method of 1-(2-dimethylaminoethyl)-1h-5-mercapto-tetrazolium
  • A kind of synthetic method of 1-(2-dimethylaminoethyl)-1h-5-mercapto-tetrazolium

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 40g of N,N-dimethylethylenediamine sodium dithiocarboxylate and 160g of reaction solvent water to a 500mL four-necked bottle in turn, mix them, and slowly add catalysts to the reaction system with stirring, that is, the mass fraction is 30% The concentration of sodium hydroxide solution is 57.3g, then 13g of sodium azide is added to the reaction system, the temperature is raised to 90°C and the temperature is kept for 16 hours. Afterwards, use 43.3g of hydrochloric acid with a mass fraction of 36% to neutralize the solution until the pH of the solution is 4, stir for 30 minutes evenly, then cool down to 8°C, filter with suction, and the filter cake is 1-(2-dimethylaminoethyl)-1H-5 -Mercapto-tetrazolium crude product, 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium crude product with 3 times the volume of recrystallization solution, that is, the mass fraction is 30% toluene / 70% water recrystallization, the recrystallization process is to completely dissolve the c...

Embodiment 2

[0028] Add 42g of N,N-dimethylethylenediamine sodium dithiocarboxylate and 210g of reaction solvent water to a 500mL four-necked bottle in turn, mix them, and slowly add catalyst to the reaction system with stirring, that is, the mass fraction is 30% The concentration of sodium hydroxide solution is 60g, then 13g of sodium azide is added to the reaction system, the temperature is raised to 85°C and the temperature is kept for 16 hours. Use 45.8g of hydrochloric acid with a mass fraction of 36% to neutralize the solution until the pH of the solution is 5, stir for 30 minutes to be uniform, then cool down to 7°C, filter with suction, and the filter cake is 1-(2-dimethylaminoethyl)-1H-5- Mercapto-tetrazolium crude product, 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium crude product with 4 times the volume of recrystallization solution, that is, the mass fraction is 35% toluene / 65 % water recrystallization, the recrystallization process is to completely dissolve the crude pro...

Embodiment 3

[0030] Add 44g of N,N-dimethylethylenediamine sodium dithiocarboxylate and 263g of reaction solvent water to a 500mL four-necked bottle in turn, mix them, and slowly add catalysts to the reaction system with stirring, that is, the mass fraction is 30% 63g of sodium hydroxide solution with a concentration of 63g, then add 13g of sodium azide to the reaction system, raise the temperature to 95°C and keep it warm for 17 hours. Afterwards, use 46.3g of sulfuric acid with a mass fraction of 50% to neutralize the solution until the pH of the solution is 5, stir for 30 minutes evenly, then cool down to 10°C, filter with suction, and the filter cake is 1-(2-dimethylaminoethyl)-1H-5 -Mercapto-tetrazolium crude product, 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium crude product is 40% toluene / 60 with the recrystallization solution of 5 times volume % water recrystallization, the recrystallization process is to completely dissolve the crude product of 1-(2-dimethylaminoethyl)-1H-5-...

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Abstract

The present invention relates to a synthetic method of 1‑(2‑dimethylaminoethyl)‑1H‑5‑mercapto‑tetrazolium, comprising the following steps: (1) using N,N‑dimethylethylenediamine Sodium dithiocarboxylate and sodium azide are raw materials, water is used as a reaction solvent, and an alkali solution is used as a catalyst. After heating and reflux, after the reaction is completed, the reaction solution is neutralized by an acid to obtain 1‑(2‑dimethyl (2) 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium crude product obtained in step (1) The crude product is recrystallized through a recrystallization solution to obtain a finished product of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium, and the recrystallization solution is a mixed solution of toluene and water. The product prepared by the invention has high purity, high yield, safer reaction process, and is a more green and environment-friendly synthesis process.

Description

technical field [0001] The invention belongs to the field of organic synthesis. Specifically, the invention relates to a synthetic method of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium. Background technique [0002] 1-(2-Dimethylaminoethyl)-1H-5-mercapto-tetrazolium is a chemical modification at the C3 position of the new-generation oral long-acting drug cefotiam. Cephalosporins are one of the fastest-growing varieties of antibiotics, and the purity of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium directly affects the cephalosporins of cefotiam axetils. Activity, exploring the synthesis of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium, reducing the synthesis cost will effectively reduce the production cost of cefotiam axetil compounds. At present, there are few introductions on the synthesis process of 1-(2-dimethylaminoethyl)-1H-5-mercapto-tetrazolium, and there are problems such as high cost, low yield and complicated equipment. [0003] About the synthe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 李石磊孙佳伟张琛杜照磊
Owner 河北凯力昂生物科技有限公司
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