Method for preparing thiabendazole

A technology of thiabendazole and benzimidazole, applied in the field of preparation of fungicides, can solve the problems of long synthesis route, high cost of raw materials, low yield and the like, and achieve the effects of short reaction time, low cost of raw materials and high yield

Inactive Publication Date: 2013-07-17
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a preparation method of thiabendazole in order to solve the technic

Method used

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Examples

Experimental program
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Effect test

specific Embodiment approach

[0028] 1. Specific embodiment one: the preparation method of thiabendazole in this embodiment is carried out according to the following steps:

[0029] 1. Synthesis of 2-(α-hydroxyethyl)benzimidazole:

[0030] Under the condition of 20-30°C, conduct the condensation reaction of o-phenylenediamine and lactic acid in dilute hydrochloric acid and reflux for 10 hours. After cooling, use ammonia water to adjust the pH value of the mixture to be greater than 7. Solids are precipitated, cooled to below 20°C, and filtered , washing the filter residue with water, drying to obtain 2-(α-hydroxyethyl) benzimidazole;

[0031] 3. Synthesis of 2-acetylbenzimidazole:

[0032] Add 2-(α-hydroxyethyl)benzimidazole, water, and magnesium sulfate in sequence in acetone, and then stir to obtain a mixed solution. Add concentrated sulfuric acid dropwise at room temperature, raise the temperature to 40°C-50°C, and add high Potassium manganate, then react at 45-55°C for 1 hour, cool to below 20°C, fil...

specific Embodiment approach 2

[0046] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the dilute hydrochloric acid in step 1 is made from concentrated hydrochloric acid and water in a mass ratio of 1:2. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0047] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that in step 1, the condensation reaction of o-phenylenediamine and lactic acid in dilute hydrochloric acid is carried out at 25°C. Others are different from the first or second specific embodiment.

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PUM

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Abstract

The invention discloses a method for preparing thiabendazole and relates to a method for preparing a bactericide. In order to solve the technical problems of high material cost, long synthetic route and low yield in the conventional method for preparing the thiabendazole, the method comprises the steps of 1, synthetizing 2-(alpha-ethoxy) benzimidazole; 2, synthetizing 2-acetylbenzimidazole; 3, synthetizing 2-(1,1-dichloro acetyl) benzimidazole; and 4, synthetizing thiabendazole. The method for preparing thiabendazole is low in material cost, simple in synthetic route, mild in reaction condition, short in reaction time, simple and convenient to operate, high in yield (high up to 87%) and suitable for industrial production; no catalyst is used; the solvent is recovered and reused; and the pollution to the environment is avoided. The method disclosed by the invention belongs to the field of preparation of the bactericide.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of a bactericide. Background technique [0002] Thiabendazole is a broad-spectrum high-efficiency fungicide. In the past ten years, it has been widely used as an antiseptic and fresh-keeping agent for fruits and other foods at home and abroad. In addition, Thiabendazole can also be used for wood preservation, leather anti-mold and anti-mold paint etc. In the prior art, there are reports in the literature that thiazole derivatives are used as intermediates to condense with aniline and its derivatives. Among these synthetic routes, some are relatively long, some have complicated technological process, some require expensive raw materials, low yield and high cost. [0003] [U.S Patent3347908] reported that thiazole derivatives were used as raw materials, but the synthesis of thiazole derivatives was difficult, with low yield and high cost...

Claims

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Application Information

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IPC IPC(8): C07D417/04
Inventor 白有银宫炜高金胜温彦鹏
Owner HEILONGJIANG UNIV
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