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Fenhexamid and analysis method thereof

A technology of fenhexamid and its synthesis method, which is applied in the field of fenhexamid and its synthesis, can solve the problems of unfavorable large-scale production of enterprises, high toxicity of organic solvents, and low yield of fenhexamid, and achieve strong reducibility , high total yield and short recovery time

Inactive Publication Date: 2018-10-23
陕西恒润化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing synthesis method of fenhexamid, the yield of fenhexamid is low, the organic solvent used in the synthesis process is highly toxic, and the safety is poor, and the recovery energy consumption is large and the time is long, resulting in the production cycle Long, high production cost, not conducive to large-scale production of enterprises

Method used

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  • Fenhexamid and analysis method thereof
  • Fenhexamid and analysis method thereof
  • Fenhexamid and analysis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0054] A synthetic method for fenhexamid, comprising the following steps:

[0055] Step 1, add 80kg of aniline to the reaction kettle, open the jacket to freeze the brine, stir at a speed of 95 rpm at 32°C, add 280kg of hydrochloric acid dropwise in the elevated tank while stirring, and drop the hydrochloric acid within 1.5 hours After adding, drop the temperature to 0°C after hydrochloric acid has been added dropwise, add dropwise the mass concentration of 50% sodium nitrite solution (58kg sodium nitrite+58kg water) in the high level tank under the condition of 2.5°C, and the sodium nitrite solution is in 2.7 hours After the internal dropwise addition, the temperature of 2.5° C. is maintained for 1 hour to obtain the diazonium salt after the dropwise addition, and the synthesis process of the diazonium salt is shown in formula (1).

[0056]

[0057] Step 2, add 130kg 2,3-dichlorophenol, 80kg sodium hydroxide and 1000kg water to the synthetic azo kettle (2,3-dichlorophenol ...

Embodiment 2

[0066] A synthetic method for fenhexamid, comprising the following steps:

[0067] Step 1, add 70kg of aniline to the reaction kettle, open the jacket to freeze the brine, stir at a speed of 95 rpm at 25°C, add 270kg of hydrochloric acid dropwise in the elevated tank while stirring, and drop the hydrochloric acid within 1.7 hours After adding the hydrochloric acid dropwise, cool down to 0°C, add 110kg of sodium nitrite solution with a mass concentration of 40% in the high level tank dropwise at 0°C, and dropwise add the sodium nitrite solution within 2.5 hours. Afterwards, heat preservation reaction at 0°C for 1.5 hours to obtain the diazonium salt.

[0068] Step 2, add 140kg 2,3-dichlorophenol, 80kg sodium hydroxide and 1100kg water to the synthetic azo kettle, 2,3-dichlorophenol is dissolved in the sodium hydroxide solution to form sodium phenolate, and water is used as the solution , stirred at a speed of 95 rpm at room temperature for 1.5 hours at a time to completely dis...

Embodiment 3

[0073] A synthetic method for fenhexamid, comprising the following steps:

[0074]Step 1, add 90kg of aniline to the reaction kettle, open the jacket to freeze the brine, stir at a speed of 95 rpm at 40°C, add 290kg of hydrochloric acid dropwise in the elevated tank while stirring, and drop the hydrochloric acid within 2 hours After the addition, drop the hydrochloric acid and drop the temperature to 0°C, add 122kg of the sodium nitrite solution with a mass concentration of 60% in the high level tank dropwise at 5°C, and drop the sodium nitrite solution within 3 hours. Afterwards, heat preservation reaction at 5°C for 2 hours to obtain diazonium salt.

[0075] Step 2, add 120kg 2,3-dichlorophenol, 80kg sodium hydroxide and 900kg water to the synthetic azo kettle, 2,3-dichlorophenol is dissolved in sodium hydroxide solution to form sodium phenolate, and water is used as the solution , stirred at a speed of 95 rpm at room temperature for 2 hours at a time to completely dissolve...

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Abstract

The invention discloses fenhexamid and an analysis method thereof. The fenhexamid is prepared from aniline, hydrochloric acid, sodium nitrite solution, 2,3-dichlorophenol, sodium hydroxide, water, ethyl alcohol, sodium hydrosulfite, 1-methyl cyclohexanoic acid, methylene dichloride, N,N-dimethyl formamide, thionyl chloride, ethyl acetate and triethylamine. The fenhexamid content reaches 98% or above, and yield reaches 86-87%; in a fenhexamid analysis process, sodium hydrosulfite adopted for azo reduction for generating 2,3-dichloro-4-hydroxylaniline is high in reducibility and quick in weak alkaline reduction reaction, and the conversion rate reaches 98% or above by cross input of sodium hydroxide and sodium hydrosulfite; pH is kept in a range of 6-7 by acid reflux after adding of sodium hydrosulfite. Fenhexamid production conditions are mild, and easiness in operation, high safety, high total yield, low cost and suitableness for large-scale production and application to enterprises are realized.

Description

technical field [0001] The invention relates to the technical field of pesticide processing, in particular to fenhexamid and a synthesis method thereof. Background technique [0002] Fenhexamid is a new type of amide systemic fungicide developed by Bayer, Germany. It is very effective in the prevention and treatment of Botrytis cinerea and Sclerotinia, and it is also effective for bacteria resistant to other chemicals. It is different from the existing fungicides. It has no cross-resistance, and is mainly used for the prevention and control of diseases including vegetables, grapes, and fruit trees. Because of its unique mechanism of action, coupled with toxicological data and ecological effects that are safe and beneficial to crops, it is an ideal drug for integrated pest management. [0003] In the existing synthesis method of fenhexamid, the yield of fenhexamid is low, the organic solvent used in the synthesis process is highly toxic, and the safety is poor, and the recov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/60C07C231/02C07C61/08C07C51/60C07C215/76C07C213/02C07C245/20C07C245/08
CPCC07C51/60C07C213/02C07C231/02C07C245/08C07C245/20C07C2601/14C07C215/76C07C61/08C07C233/60
Inventor 樊明李仓珍谌敦国晁六民王建桥尹炜新
Owner 陕西恒润化学工业有限公司