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Synthesis method of thiodicarb

A technology of thiodimethomyl and synthetic methods, applied in the direction of organic chemistry, etc., can solve problems such as product quality impact, insufficient impurity control, easy to block pipelines, etc., to achieve improved selectivity and product quality, simple process operation, and improved selection sexual effect

Active Publication Date: 2021-05-11
湖南海利常德农药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Due to the increasingly severe situation of the global environment, in order to further reduce the impact of chemical pesticides on the environment and produce high-quality pesticides, reducing the content of non-active ingredients in pesticides is also one of the current development directions of pesticides. Patent CN108047106A improves the traditional process and reduces the product cost. The thiodimethomyl isomer impurity in thiodicarb improves the product purity, but the impurity control in thiodicarb is not enough, which affects the product quality, and it is easy to block in the large-scale production process pipeline, so the process still needs to be further improved

Method used

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  • Synthesis method of thiodicarb

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Effect test

Embodiment 1

[0032] A kind of synthetic method of thiodicarb of the present invention comprises:

[0033] Add 244.00 g of pyridine and 0.08 g of 18-crown-6 into a 1000 mL four-necked flask equipped with mechanical stirring, a thermometer, and a constant pressure dropping funnel. Seal the reaction system, lower the temperature to -5°C, first dropwise add 1 / 3 of 66.98g sulfur dichloride (calculated as 83% in mass content), after the addition of sulfur dichloride is completed, slowly pass chlorine gas, and then gradually increase the temperature In the process of reaching 15°C, the pyridine solution of methomyl (162.20g methomyl dissolved in 243.00g pyridine) and the remaining sulfur dichloride were added dropwise at the same time, and the dripping was completed within 4 hours, and the chlorine gas flow was stopped after the addition was completed. A total of 0.67g of chlorine gas was passed into the reaction solution, and then kept at 15°C for 4 hours. After the reaction was completed, 285.0...

Embodiment 2

[0036] A kind of synthetic method of thiodicarb of the present invention comprises:

[0037] Add 487.00 g of pyridine and 0.81 g of 18-crown-6 into a 1000 mL four-necked flask equipped with mechanical stirring, a thermometer, and a constant pressure dropping funnel. Seal the reaction system, drop the temperature to 5°C, add dropwise 1 / 2 of 74.43g sulfur dichloride (mass content is calculated according to 83%), after the sulfur dichloride has been added dropwise, start slowly flowing chlorine gas, and then gradually heat up to In the process of 25 DEG C, add dropwise the pyridine solution of methomyl (162.20g methomyl is dissolved in 324.00g pyridine to gain) and remaining sulfur dichloride simultaneously, dropwise finish within 6 hours, stop feeding chlorine gas after dropwise addition, a total of Introduce 2.23g of chlorine gas into the reaction solution, and then keep it warm at 25°C for 6 hours. After the reaction, add 285.00g of methanol to the reaction solution for quench...

Embodiment 3

[0040] A kind of synthetic method of thiodicarb of the present invention comprises:

[0041]Add 373.06 g of pyridine and 0.65 g of 18-crown-6 into a 1000 mL four-neck flask equipped with mechanical stirring, a thermometer, and a constant pressure dropping funnel. Seal the reaction system, drop the temperature to 5°C, add 1 / 2 of 70.70g sulfur dichloride (calculated according to 83% mass content) dropwise, after the sulfur dichloride has been added dropwise, start slowly flowing chlorine gas, and then gradually heat up to In the process of 20 DEG C, dropwise the pyridine solution of methomyl (162.20g methomyl is dissolved in 275.74g pyridine and obtain) and remaining sulfur dichloride simultaneously, dropwise finish within 5 hours, stop logical chlorine gas after dropwise addition, altogether Introduce 1.27g of chlorine gas into the reaction solution, and then keep it warm at 20°C for 5 hours. After the reaction, add 285.00g of methanol to the reaction solution for quenching. Du...

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Abstract

The invention discloses a synthesis method of thiodicarb, which comprises the following steps: (1) dividing a solvent into two parts, dissolving methomyl in one of the two parts to obtain a methomyl solution, and dissolving 18-crown ether-6 in the other part of the mixture to obtain a solution of the 18-crown-6; and (2) under a closed condition, dropwise adding a part of sulfur dichloride into the 18-crown-6 solution, after dropwise adding is completed, dropwise adding the residual sulfur dichloride to react with the methomyl solution, and after dropwise adding is completed, continuing to carry out heat preservation reaction to obtain the thiodicarb. The method is high in reaction selectivity, by-products are reduced, the obtained product is high in purity and yield, and meanwhile, the problem that a pipeline is easily blocked in the production process can be effectively solved. The method is simple in process operation and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of pesticide compound synthesis, and in particular relates to a synthesis method of thiodicarb. Background technique [0002] Thiodicarb (thiodicarb for short), English common name thiodicarb, also known as Lavein, is a second-generation carbamate insecticide, which is further improved on the basis of methomyl and has a low One of the poisoned derivatives, that is, two methomyl molecules are connected through a thioether chain to form a biscarbamate, and the toxicity is only about one tenth of that of methomyl. It is a high-efficiency, broad-spectrum, low toxicity, Systemic stomach poisonous insecticide. The product was developed simultaneously by United Carbide and Ciba-Geigy in 1977 and put into production in 1984. So far, it has been registered in more than 30 countries in the world, with an annual sales volume of thousands of tons. The drug is widely used in crops such as cotton, vegetables, fruit tre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/08
CPCC07C381/08
Inventor 虞孝云席树文徐健刘双瑾彭长春杨自力周子斌丁德军黄爱国
Owner 湖南海利常德农药化工有限公司
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