A kind of technique of synthetic omethoate important intermediate oxathion

A technology of oxythiophosphate and oxythiophosphate, which is applied in the field of synthesizing omethoate important intermediate oxythiophosphate, can solve the problems of increasing the chance of meeting main and by-products, large heat release of the system, difficult temperature operation and the like , to reduce the chance of molecular collision, control the reaction temperature, and achieve the effect of obvious process advantages

Active Publication Date: 2020-12-25
兰博尔开封科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional process of this reaction, water needs to be added, and the reaction is carried out at 65°C. The entire process environment is particularly conducive to the dissolution of ammonium chloride in the crude ester system, thus resulting in a large amount of exothermic heat in the system, difficulties for employees to operate the temperature, and increased The progress of the side reaction increases the chance of meeting the main by-products to a greater extent and reduces the yield of this step

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of technique of synthesizing the important intermediate of omethoate: drop into 900kg methyl chloroacetate, 500L ammonium sulfophosphate, 2.5kg triethylamine successively in reactor, open stirring, steam valve, when temperature rises to Close the steam valve at 45°C and keep warm at 45°C for 3 hours. After the heat preservation is over, open the cooling water valve to cool down the material. When the temperature drops to 30°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride. The filtrate thrown out is oxygen sulfur Phosphate crude ester, carry out tertiary drying and precipitating the crude phosphion ester ester, control the precipitating temperature at 100-130°C, control the vacuum below -0.095MPa, remove methyl chloroacetate, and obtain phosphion sulfonate essence Esters; the centrifuged ammonium chloride is dried and sold as a by-product.

[0026] The desiccant used for drying is 3A molecular sieve, and ...

Embodiment 2

[0029] A kind of technique of synthetic omethoate important intermediate oxothioate: drop into 1200kg methyl chloroacetate, 900L ammonium sulfophosphate, 3.5kg triethylamine successively in reactor, open stirring, steam valve, when temperature rises to Close the steam valve at 55°C, keep warm at 55°C for 3 hours, open the cooling water valve to cool the material after the heat preservation is over, and discharge the material when the temperature drops to 30°C, the material is subjected to centrifugal separation of ammonium chloride, and the filtrate thrown out is oxygen sulfur Phosphate crude ester, carry out tertiary drying and precipitating the crude phosphion ester ester, control the precipitating temperature at 100-130°C, control the vacuum below -0.095MPa, remove methyl chloroacetate, and obtain phosphion sulfonate essence Esters; the centrifuged ammonium chloride is dried and sold as a by-product.

[0030] The desiccant used for drying is 3A molecular sieve, and the weig...

Embodiment 3

[0033] A process for synthesizing the important intermediate oxymethoate: drop into 1000kg methyl chloroacetate, 700L ammonium sulfophosphate, 4kg triethylamine successively in the reactor, open the stirring and steam valve, when the temperature rises to 50 Close the steam valve at 50°C, keep warm at 50°C for 3 hours, open the cooling water valve to cool the material after the heat preservation is over, and discharge the material when the temperature drops to 30°C, the material is subjected to centrifugal separation of ammonium chloride, and the filtrate thrown out is oxysulfon For the crude ester, carry out tertiary drying and precipitation of the crude ester of oxythiophosphine, control the precipitation temperature at 100-130°C, control the vacuum below -0.095MPa, remove methyl chloroacetate, and obtain the refined oxothionate ; The centrifuged ammonium chloride is sold as a by-product after being dried.

[0034] The desiccant used for drying is 3A molecular sieve, and the ...

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PUM

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Abstract

The invention discloses a new process for synthesizing an important intermediate oxinothiophospholipid of omethoate. The process comprises the steps of adopting an anhydrous system to synthesize the oxinothiophospholipid, drying an oxinothiophospholipid coarse ester, and preparing the oxinothiophospholipid. According to the anhydrous reaction process technology provided by the invention, the reaction environment is maximally improved, the progress of main reaction is improved, the adverse factors brought by solid-liquid reaction are solved, the hydrolysis is reduced, the reaction yield is improved, and a salt-containing compound is convenient to post-treat. By using the new process provided by the invention, the purity of the oxinothiophospholipid can reach to more than 89 percent, the yield of the oxinothiophospholipid can reach to more than 86 percent, the purity of ammonium chloride can reach to more than 99 percent, and the ammonium chloride can be directly used as a by-product first-grade product for sales. Compared with the traditional process, the overall effect is greatly improved, and the social benefit and the economic benefit are great.

Description

technical field [0001] The invention relates to a process for synthesizing an important intermediate of omethoate, oxathion, and belongs to the technical field of intermediate synthesis. Background technique [0002] There are many side reactions in solid-liquid organic synthesis reactions, and the occurrence of side reactions has more or less influence on the main reaction, such as: affecting the progress of the main reaction, affecting the content and yield of the main product, etc. In the process of solid-liquid organic synthesis, salt-containing by-products are the most common. How to solve the problem of salt-containing by-products in the process of solid-liquid organic synthesis has been a research topic for many organic synthesis researchers. [0003] The oxymethoate reaction in the synthesis of omethoate plays a connecting role in the whole process. And the generation of by-product ammonium chloride is also inevitable in this reaction. In the traditional process of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/48
CPCC07F9/4816
Inventor 常书浩董光霞霍二福刘沛敬李晓琼乔晓会李红金孙宝臣刘宏勋汤肖倩
Owner 兰博尔开封科技有限公司
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