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Probenazole low-toxicity bactericide and preparation method thereof

A technology of thiabendazole and bactericide, which is applied in the field of low toxicity bactericide thiabendazole and its preparation, can solve the problems of potential safety hazards, increased cost and risk, and expensive raw materials of pyruvic acid, etc., so as to improve the conversion rate and yield , Simplify the production process and reduce the effect of unsafe factors

Inactive Publication Date: 2012-02-29
SHANDONG MEI LUO FU AGRI POLYTRON TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) The escape of bromine and HBr increases the cost and danger of production;
[0007] (2) The raw material of pyruvic acid is more expensive;
[0008] (3) adopting liquefied ammonia in the reaction is raw material, easily produces potential safety hazard;
[0010] (5)SOCl 2 Extremely unstable in contact with water, easily hydrolyzed to generate SO 2 and HCl, thereby creating a safety hazard
As the level of science and technology improves, as a classic and efficient pesticide, the new synthesis process of thiabendazole has been designed and perfected, but the key steps of the new technology are still in the hands of foreign pesticide production companies. No breakthrough has been made, and the domestic market demand can only be met by importing thiabendazole technical

Method used

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  • Probenazole low-toxicity bactericide and preparation method thereof
  • Probenazole low-toxicity bactericide and preparation method thereof
  • Probenazole low-toxicity bactericide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A preparation method of low-toxicity bactericide thiabendazole, the steps are as follows:

[0043] (1) 27.2g of bromine was dissolved in 40ml of ethanol while cooling in a water bath to obtain solution A;

[0044] (2) Add 8.8 g of pyruvic acid into 1 ml of concentrated sulfuric acid, heat to 50° C., then add the solution A prepared in step (1), and react for 2.0 h to obtain mixture I;

[0045] (3) Add 5g P 2 S 5 Add 5g of formamide into 213.5g of 2-methyltetrahydrofuran, and react at 50°C for 1.5h to obtain solution II;

[0046] (4) Add the mixture I prepared in step (2) to solution II, raise the temperature to 70°C, react for 4h, cool to room temperature, let stand for 10h, filter to collect the precipitate, and dry at 60°C to obtain thiazole-4- ethyl carboxylate;

[0047] (5) Add 2.1 g of o-phenylenediamine and 5 g of ethyl thiazole-4-carboxylate prepared in step (4) to 50 g of polyphosphoric acid, mix well and heat to 150° C. under the protection of nitrogen, and...

Embodiment 2

[0070] A preparation method of low-toxicity bactericide thiabendazole, the steps are as follows:

[0071] (1) 22g of bromine was dissolved in 40ml of ethanol while cooling in a water bath to obtain solution A;

[0072] (2) Add 8.8 g of pyruvic acid into 1 ml of concentrated sulfuric acid, heat to 50° C., then add the solution A prepared in step (1), and react for 2.0 h to obtain mixture I;

[0073] (3) Add 4g P 2 S 5 Add 5g of formamide into 213.5g of 2-methyltetrahydrofuran, and react at 50°C for 1.5h to obtain solution II;

[0074] (4) Add the mixture I prepared in step (2) to solution II, raise the temperature to 70°C, react for 4h, cool to room temperature, let stand for 10h, filter to collect the precipitate, and dry at 60°C to obtain thiazole-4- ethyl carboxylate;

[0075] (5) Add 1.5 g of o-phenylenediamine and 5 g of ethyl thiazole-4-carboxylate prepared in step (4) to 45 g of polyphosphoric acid, mix well and heat to 150° C. under the protection of nitrogen, and r...

Embodiment 3

[0079] A preparation method of low-toxicity bactericide thiabendazole, the steps are as follows:

[0080] (1) Dissolve 30.8g of bromine in 40ml of ethanol while cooling in a water bath to obtain solution A;

[0081] (2) Add 8.8 g of pyruvic acid into 1 ml of concentrated sulfuric acid, heat to 50° C., then add the solution A prepared in step (1), and react for 2.0 h to obtain mixture I;

[0082] (3) Add 6g P 2 S 5 Add 5ml of formamide into 213.5g of 2-methyltetrahydrofuran and react at 50°C for 1.5h to obtain solution II;

[0083] (4) Add the mixture I prepared in step (2) to solution II, raise the temperature to 70°C, react for 4h, cool to room temperature, let stand for 10h, filter to collect the precipitate, and dry at 60°C to obtain thiazole-4- ethyl carboxylate;

[0084] (5) Add 3.0 g of o-phenylenediamine and 5 g of ethyl thiazole-4-carboxylate prepared in step (4) to 55 g of polyphosphoric acid, mix well and heat to 150° C. under the protection of nitrogen, and reac...

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Abstract

The invention relates to a probenazole low-toxicity bactericide and a preparation method thereof, and belongs to the technical field of pesticide. The preparation method comprises the following steps: dissolving bromine in ethanol to obtain solution A; adding pyruvic acid into concentrated sulfuric acid, adding the solution A and obtaining a mixture I; adding P2S5 and formamide into 2-methyltetrahydrofuran to obtain solution II; adding the mixture I into the solution II, filtering, collecting precipitate, drying the precipitate, and obtaining thiazole-4-carboxylate; adding o-phenylenediamine and thiazole-4-carboxylate into polyphosphoric acid, reacting, mixing with water, filtering, drying and obtaining coarse probenazole; and adding coarse probenazole in absolute ethanol, adding active carbon, filtering, cooling filtrate to room temperature, filtering, drying, precipitating and obtaining probenazole. In the invention, bromine is dissolved in absolute ethanol and reacted, the operability of bromine is improved, the volatilization of a hydrogen bromide gas is slowed, the subsequent absorption process is continuous and controllable, and the unsafe factors in the production are reduced.

Description

technical field [0001] The invention relates to a low-toxicity fungicide thiabendazole and a preparation method thereof, belonging to the technical field of pesticides. Background technique [0002] Thiabendazole (TBZ) is commonly known as Tecdo, Tibendazole, Thiobendazole, Thiabendazole, and its chemical name is 2-(4-thiazolyl)-benzimidazole, referred to as TBZ. It is a white crystal, which is resistant to heat and acid. , Alkali is extremely stable. It is an anti-parasitic drug invented in the United States in the early 1960s. It has the ability to conduct systemically to the apex, but not to the base. Thiabendazole has a long-lasting effect, has cross-resistance with benzimidazole fungicides, and has inhibitory activity against Ascomycetes, Basidiomycetes and Deuteromycetes. It is a high-efficiency, broad-spectrum, international universal fungicide. It is used for processing 42% thiabendazole suspension concentrate, 60% thiabendazole wettable powder, 3% thiabendazole s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/04
Inventor 李杜李红云褚荣花耿伟刘玉清王玉军李苗李玲李丽
Owner SHANDONG MEI LUO FU AGRI POLYTRON TECH
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