New process for synthetizing lythidathion

A technology of thiazophos and a new process, applied in the chemical field, can solve the problem of low yield of thiazophos, and achieve the effect of high product yield and low synthesis cost

Inactive Publication Date: 2012-10-03
山东华阳农药化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problem that the yield of thiazole phosphorus is not high in the existing process, the...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 114g of cysteamine hydrochloride, 75g of urea and 100ml of phenol into the reaction flask at the same time, stir, heat up to 80°C to melt, keep warm at 140°C for 1.5 hours, filter at 60°C, the filter cake is ammonium chloride, and the filtrate is desolvated, which is Thiazolidinone, the yield is 101g, the content is 97%, and the yield is 95%.

[0022] In a four-necked flask equipped with an electric stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, sequentially add 400 mL of tert-butanol, 76 g of thiourea, and 5 g of DTEBA and stir to raise the temperature to 40 ° C, and dropwise add 137 g of brominated sec-butane , The dropwise addition time was about 0.5 hours, and then kept stirring for 1.5 hours. Under stirring state, dropwise add 266g of 30% liquid caustic soda, heat, control temperature at 60 ℃, drop and finish cooling to 25 ℃, layering, the oily thing of upper layer is sec-butyl mercaptan, yield is 87g, content 99%, yield Th...

Embodiment 2

[0027] Add 114kg of cysteamine hydrochloride, 75kg of urea and 100L of phenol into the reaction kettle at the same time, stir, heat up to 80°C to melt, continue to keep warm at 160°C for 1.5 hours, filter at 50°C, the filter cake is ammonium chloride, and the filtrate is desolvated, namely It is thiazolidinone, the yield is 102kg, the content is 97%, and the yield is 96%.

[0028] In a reaction kettle equipped with an electric stirrer, a thermometer, and a reflux condenser, sequentially add 400 L of dioxane, 76 kg of thiourea, and 5 kg of CTEBA and stir to raise the temperature to 40° C. The addition time is about 0.5 hours, and then the temperature is kept under stirring for 1.5 hours. Under stirring state, dropwise add 266kg of 30% liquid caustic soda, heat, control temperature at 60 ℃, drop and finish cooling to 25 ℃, layering, the oily thing of upper layer is sec-butyl mercaptan, yield is 88kg, content 99%, yield The rate is 96.8%.

[0029] Add 400L of toluene and 72kg o...

Embodiment 3

[0033] Add 228g of cysteamine hydrochloride, 150g of urea and 200ml of phenol into the reaction flask at the same time, stir, heat up to 80°C to melt, keep warm at 150°C for 1.5 hours, filter at 60°C, the filter cake is ammonium chloride, and the filtrate is desolvated, which is Thiazolidinone, the yield is 204g, the content is 96.5%, and the yield is 95.6%.

[0034] In a four-necked flask equipped with an electric stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, sequentially add 800 mL of tert-butanol, 152 g of thiourea, and 10 g of DTEBA, stir to raise the temperature to 40 ° C, and dropwise add 274 g of brominated sec-butane , The dropwise addition time was about 0.5 hours, and then kept stirring for 1.5 hours. Under stirring state, add 532g of 30% sodium hydroxide solution dropwise, heat, control the temperature at 60°C, drop the temperature to 25°C after dropping, separate layers, the oil in the upper layer is sec-butylmercaptan, the yie...

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Abstract

The invention discloses a new process for synthetizing lythidathion. Mercaptamine and urea are used as initial materials to simply obtain lythidathion active compound of which the content is more than 98.0% by reactions of thiazolidone synthesis, sec-butyl mercaptan synthesis, sec-butyl phosphoryl chloride synthesis, lythidathion synthesis and the like.

Description

technical field [0001] The invention relates to a synthesis process of thiazole phosphorus, which belongs to the field of chemistry. Background technique [0002] Thiazophos is a novel, efficient and broad-spectrum non-fumigation organophosphorus insecticide and nematicide developed by Ishihara Corporation of Japan, and has been put on the market in Japan and many other countries. Preliminary studies have shown that thiazophos has a systemic transport effect in plants and has broad-spectrum activity against plant parasitic nematodes and pests. Plant parasitic nematodes harm many important crops, and the biological and physical and chemical properties of thiazophos are very suitable for soil surface application, so it becomes an ideal agent for controlling plant parasitic nematodes. At present, most of the pesticides widely used in the control of nematodes in China are highly toxic or highly toxic, such as carbofuran, carbosulfan, aldicarb, protamifos, and gramphos. Thiazop...

Claims

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Application Information

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IPC IPC(8): C07F9/6539
Inventor 薛红伟宋东升王同涛孔斌刘自友闫新华王凤芝李振兴冯训娟
Owner 山东华阳农药化工集团有限公司
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