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Preparation method of tinidazole

A technology for tinidazole and nitroimidazole, applied in the field of preparation of tinidazole, can solve the problems of increasing manufacturing cost, large waste liquid and the like, and achieve the effects of reducing separation cost, reducing the amount of three wastes, and reducing volatilization

Inactive Publication Date: 2017-05-10
HUBEI HONGYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the problem that it exists is that it improves the yield of tinidazole by neutralizing the acid with lye, will produce a large amount of waste liquid, also increased manufacturing cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Add 20g of β-hydroxyethyl sulfide and 40g of 2-methyl-5-nitroimidazole into a 250ml three-necked flask, then add 40ml of xylene, heat up, and add 10g of solid super acid at 45°C , stir evenly, and then heat up to 85±2°C for 3~5 hours. After the heat preservation is completed, cool down to room temperature, filter, take the organic layer, and wash the filtered solid part with water to retain the washing solution;

[0023] 2. Turn on the stirring, add 17g of hydrogen peroxide to the mixture of the organic layer washing liquid, and pass in air, and control the flow rate of the air to 15ml / min; at the same time, slowly raise the temperature to 55~60°C, keep it warm for 1 hour, and cool down The crude product of tinidazole was obtained by filtration. Tinidazole crude product adopts 7 times of purified water to dissolve and add 0.8% active carbon decolorization 30min of tinidazole crude product weight, filter while hot, filtrate cooling crystallization, filter, dry to obt...

Embodiment 2

[0026] 1. Add 20g of β-hydroxyethyl sulfide and 36.9g of 2-methyl-5-nitroimidazole into a 250ml three-necked flask, then add 40ml of xylene, heat up, and add solid super acid at 45°C 12.3g, stir evenly, then raise the temperature to 85±2℃ and keep it for 3~5 hours. After the heat preservation is completed, cool down to room temperature, filter, take the organic layer, and wash the filtered solid part with water to retain the washing liquid;

[0027] Start stirring, add 14.5g of hydrogen peroxide to the mixture of the organic layer washing solution, and pass in air, control the flow rate of the air to 15ml / min; at the same time, slowly raise the temperature to 55~60°C, keep it warm for 1 hour, cool and filter The crude product of tinidazole was obtained. The tinidazole crude product was dissolved in 6 times of purified water and added 1.2% of tinidazole crude product weight for decolorization with activated carbon for 30min, filtered while hot, the filtrate cooled and crystall...

Embodiment 3

[0029] 1. Add 20g of β-hydroxyethyl sulfide and 42.5g of 2-methyl-5-nitroimidazole into a 250ml three-necked flask, then add 40ml of xylene, heat up, and add 8.5g of solid at 45°C Super acid, stir evenly, then raise the temperature to 85±2°C and keep it for 3~5 hours. After the heat preservation is completed, cool down to room temperature, filter, take the organic layer, and wash the filtered solid part with water to retain the washing liquid;

[0030] 2. Turn on the stirring, add 20g of hydrogen peroxide to the mixture of the organic layer washing liquid, and pass in air, and control the flow rate of the air to 15ml / min; at the same time, slowly raise the temperature to 55~60°C, keep it warm for 1 hour, and cool down The crude product of tinidazole was obtained by filtration. Tinidazole crude product adopts purified water to dissolve and add 1% gac decolorization 30min of tinidazole crude product weight, filter while hot, filtrate cooling crystallization, filter, dry to obta...

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PUM

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Abstract

The invention belongs to the field of chemical pharmacy, and particularly relates to a preparation method of tinidazole. The method includes steps of applying beta- hydroxy ethyl thioether and 2-methyl-5- nitroimidazole as raw material, using xylene series as the solvent; performing condensation reaction under the function of solid superacid; water-washing and acquiring the condensate 1-(beta- ethion ethyl)-2-methyl-5-nitroimidazole; then oxidizing the condensate 1-(beta- ethion ethyl)-2-methyl-5-nitroimidazole under the combined action of hydrogen peroxide and air, and acquiring the crude product of tinidazole. The method needs not the alkali liquid to neutralize condensation reaction liquid, thus the preparation steps of tinidazole are shortened; the preparation method saves cost and reduces three wastes.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, in particular to a preparation method of tinidazole. Background technique [0002] Tinidazole is a highly effective anti-amoeba and anti-anaerobe drug. Compared with the traditional anti-anaerobe drug metronidazole, it has the advantages of good drug effect and small side effects. [0003] Regarding the preparation method of tinidazole, current bibliographical reports generally use β-hydroxyethyl sulfide and 2-methyl-5-nitroimidazole as raw materials, methyl isobutyl ketone as solvent, and condensation reaction under Lewis acid catalysis The condensate 1-(β-ethylthioethyl)-2-methyl-5-nitroimidazole is obtained, and then oxidized with about 30% hydrogen peroxide under acidic conditions to obtain the desired product—tinidazole. The reaction steps of this process require four steps, and there are mainly disadvantages such as a large number of raw materials required, large pollution at the operation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/94
CPCC07D233/94
Inventor 方高方耀吕智国丰光俊徐双喜邓支华晏浩哲
Owner HUBEI HONGYUAN PHARMA
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