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Catalyst-free synthetic method of profenofos original medicine

A synthesis method and profenofos technology are applied in the field of catalyst-free profenofos technical synthesis to achieve the effects of ensuring health, low cost and reducing occupational hazard factors

Inactive Publication Date: 2019-06-04
山东科源化工有限公司
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Problems solved by technology

[0005] The purpose of the present invention is to provide a catalyst-free profenofos original drug synthesis method, the present invention can mainly solve the use problem of dimethylformamide, in the synthesis process, no longer use the catalyst, and ensure the synthesis of profenofos

Method used

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  • Catalyst-free synthetic method of profenofos original medicine

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Embodiment 1

[0020] A kind of catalyst-free profenofos former drug synthetic method, comprises the steps:

[0021] 1). O, O-diethyl-O-(2-chloro-4-bromophenyl)-phosphorothioate and trimethylamine are heated under reflux to undergo a dealkylation reaction, and the trimethylamine is removed by rotary evaporation under reduced pressure to obtain Onium salt intermediate;

[0022] 2). Add water and bromopropane to the onium salt intermediate obtained in the previous step, and use nitrogen pressure in a closed container to carry out transposition synthesis;

[0023] 3). The product obtained in step 2) is allowed to stand for stratification, and the water in the upper layer is removed. The obtained product is the crude profenofos product. The crude product of profenofos is washed with water, and the solvent is distilled off to obtain the profenofos product.

[0024] The reaction temperature of O,O-diethyl-O-(2-chloro-4-bromophenyl)-phosphorothioate and trimethylamine in step 1) is 60±5°C.

[002...

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Abstract

The invention discloses a catalyst-free synthetic method of a profenofos original medicine, and relates to the field of preparation of the profenofos original medicine, in the synthesis process, a catalyst is not used, a reaction kettle is completely sealed, nitrogen is introduced to increase the gas-phase pressure to 0.1-0.3 MPa, the volatilization of bromopropane is reduced, and the concentration of the bromopropane in a reaction liquid is maintained, so that the reaction is carried out in the positive reaction direction, the conversion rate of an onium salt and the bromopropane is ensured,the 96% profenofos original medicine can be obtained by water washing, desolventizing and other post-treatment, no DMF (dimethyl formamide) is used as a catalyst in the synthetic method of the profenofos, and the effect of reducing occupational hazard factors is realized.

Description

technical field [0001] The invention relates to the field of profenofos technical manufacture, in particular to a method for synthesizing the catalyst-free profenofos technical. Background technique [0002] Profenofos is a common organophosphorus insecticide. Dimethylformamide (DMF) is generally used as a phase transfer catalyst for catalytic transposition in the synthesis of domestic profenofos original drug. Onium salt, after removing excess trimethylamine, add water and bromopropane to carry out catalytic transposition synthesis under 65-72°C temperature and reflux conditions using dimethylformamide (DMF) as a phase transfer catalyst. Generally, profenofosin is synthesized The content is 92-96%. [0003] For example, in the invention patent of the preparation method of high-purity profenofos with the publication number CN102617636A, it is disclosed that the synthesis steps of the original drug of profenofos including the use of dimethylformamide: 1) bromination; 2) recr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/18
Inventor 刘旭东邱瑞栋张明伟李烨
Owner 山东科源化工有限公司
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