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Method for synthesizing isoxadifen-ethyl intermediate 2-chloro-2-hydroxyiminoacetic acid ethyl ester

A technology of ethyl chloroacetoacetate and ethyl ethyl acetate is applied in the field of synthesizing ethyl chlorooximoethyl acetate, an intermediate of bisoxazole, and can solve the problems of low production efficiency, high production cost of bisoxazole, The problems of poor reactivity and stability can reduce production difficulty and production cost, improve work efficiency and production quality, and improve chemical reactivity.

Pending Publication Date: 2021-06-18
河南佰研生物科技有限公司
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  • Abstract
  • Description
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Problems solved by technology

[0002] Chloroxime ethyl acetate is widely used in various types of biological agents, and the amount of use is huge, but it has serious toxic and side effects and relatively high production requirements, which on the one hand leads to the current chloroxime The production process of ethyl chlorooximyloacetate is complicated, the production difficulty is large and the production efficiency is relatively low, and the reactivity and stability of various raw materials used to prepare ethyl chlorooximinoacetate are poor, which affects the production of ethyl chlorooximinoacetate production efficiency and quality; on the other hand, the chemical bond and crystal structure of the ethyl chlorooximyloacetate product obtained by the traditional production process of ethyl chlorooximyloacetate are relatively stable, which leads to the When ethyl acetate is used to prepare isoxadifen, the reaction efficiency of isoxadifen is low, which leads to high production cost and low production efficiency of isoxadifen

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  • Method for synthesizing isoxadifen-ethyl intermediate 2-chloro-2-hydroxyiminoacetic acid ethyl ester

Examples

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Effect test

Embodiment 1

[0020] A method for synthesizing isoxadifen acid intermediate chlorooximino ethyl acetate, comprising the following steps:

[0021] S1, mother liquor prefabrication, first seal the reactor to form a closed cavity structure, then adjust the temperature of the reactor to 5°C, and pass inert gas into the reactor to replace the oxygen in the reactor, and make the oxygen content in the reactor is 0, and the air pressure is 0.1 Mpa; finally, ethyl acetate is added to the reactor, and left to stand for 5 minutes until the temperature of the ethyl acetate is consistent with the temperature of the reactor, and the ethyl acetate is kept insulated;

[0022] S2, prepare ethyl chloroacetoacetate, add sulfuryl chloride dropwise to the ethyl acetate after S1 temperature adjustment at a uniform speed, wherein the total amount of sulfuryl chloride added dropwise is 1.1 times of the total amount of ethyl acetate in the S1 step, and react The mixed solution in the kettle was stirred at constant ...

Embodiment 2

[0030] A method for synthesizing isoxadifen acid intermediate chlorooximino ethyl acetate, comprising the following steps:

[0031] S1, mother liquor prefabrication, first seal the reactor to form a closed cavity structure, then adjust the temperature of the reactor to 15°C, and pass nitrogen into the reactor to replace the oxygen in the reactor, and make the oxygen content in the reactor be 3%, and the air pressure is 0.35 Mpa; finally ethyl acetate is added to the reactor, and left to stand for 15 minutes until the temperature of the ethyl acetate is consistent with the temperature of the reactor, and the ethyl acetate is kept insulated;

[0032] S2, prepare ethyl chloroacetoacetate, add sulfuryl chloride dropwise to the ethyl acetate after S1 temperature adjustment at a uniform speed, wherein the total amount of sulfuryl chloride added dropwise is 1.5 times of the total amount of ethyl acetate in the S1 step, and react The mixed solution in the kettle was stirred at constan...

Embodiment 3

[0038] A method for synthesizing isoxadifen acid intermediate chlorooximino ethyl acetate, comprising the following steps:

[0039] S1, mother liquor prefabrication, first seal the reactor to form a closed cavity structure, then adjust the temperature of the reactor to 10°C, and pass argon into the reactor to replace the oxygen in the reactor, and make the oxygen content in the reactor 2%, and the air pressure is 0.25 Mpa; finally ethyl acetate is added to the reactor, and left to stand for 8 minutes until the temperature of the ethyl acetate is consistent with the temperature of the reactor, and the ethyl acetate is kept insulated;

[0040]S2, prepare ethyl chloroacetoacetate, add sulfuryl chloride dropwise to the ethyl acetate after S1 temperature adjustment at a uniform speed, wherein the total amount of sulfuryl chloride added dropwise is 1.3 times of the total amount of ethyl acetate in the S1 step, and react The mixed solution in the kettle was stirred at constant temper...

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Abstract

The invention provides a method for synthesizing an isoxadifen-ethyl intermediate 2-chloro-2-hydroxyiminoacetic acid ethyl ester. The method comprises the steps of mother liquor prefabrication, ethyl chloroacetoacetate preparation and synthesis reaction. Compared with the traditional 2-chloro-2-hydroxyiminoacetic acid ethyl ester, the method has the advantages that the production process is effectively simplified, the working efficiency of reaction operation of each raw material is improved, the stability of material reaction is improved, the production difficulty and the production cost are effectively reduced. The environment pollution caused by the 2-chloro-2-hydroxyiminoacetic acid ethyl ester and the raw materials for preparing the 2-chloro-2-hydroxyiminoacetic acid ethyl ester can be effectively prevented, and the working safety of production operation is improved; and meanwhile, the chemical reaction activity of 2-chloro-2-hydroxyiminoacetic acid ethyl ester is greatly improved, the working efficiency and production quality of subsequent preparation of isoxadifen-ethyl can be effectively improved, and the production cost of isoxadifen-ethyl is reduced.

Description

technical field [0001] The invention relates to a method for synthesizing ethyl chlorooximinoacetate, an intermediate of isoxadifen, and belongs to the technical field of chemical industry. Background technique [0002] Chloroxime ethyl acetate is widely used in various types of biological agents, and the amount of use is huge, but it has serious toxic and side effects and relatively high production requirements, which on the one hand leads to the current chloroxime The production process of ethyl chlorooximyloacetate is complicated, the production difficulty is large and the production efficiency is relatively low, and the reactivity and stability of various raw materials used to prepare ethyl chlorooximinoacetate are poor, which affects the production of ethyl chlorooximinoacetate production efficiency and quality; on the other hand, the chemical bond and crystal structure of the ethyl chlorooximyloacetate product obtained by the traditional production process of ethyl chl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/38C07C67/307C07C69/72
CPCC07C249/04C07C67/307C07C69/72C07C251/38
Inventor 鞠超袁坤朋刘琼洋
Owner 河南佰研生物科技有限公司
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