Method for synthesizing penoxsulam

A technology of penoxsulam and difluoroethoxy, which is applied in the field of preparation of penoxsulam, can solve the problems of difficult treatment of the three wastes, involve many dangerous raw materials, and low product yield, so as to improve the reaction yield. efficiency and product quality, easy recovery and application, and the effect of optimizing reaction conditions

Inactive Publication Date: 2018-01-19
湖北犇星农化有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction time of this process is as long as about 9 days, the product yield is low, and it involves many dangerous raw materials, so it is difficult to treat the three wastes

Method used

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  • Method for synthesizing penoxsulam

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Effect test

Embodiment 1

[0048] The present invention relates to a kind of preparation method of penoxsulam, comprising the following steps:

[0049] A. Synthesis of intermediate products

[0050] (1) Dissolve 0.5mol trimethylchlorosilane and 0.5mol sodium iodide in a three-neck flask filled with 400ml of anhydrous acetonitrile, and stir evenly; the temperature during the feeding process is controlled at 0-40°C;

[0051] (2) At room temperature, mix 0.5mol 5,8-dimethoxy-[1,2,4]triazol[1,5-c]pyrimidin-2-amine with 0.5mol triethylamine in a beaker Stir to mix;

[0052] (3) Add the mixed triethylamine solution dropwise to the three-necked flask being stirred, and stir and react for 4 hours after the dropwise addition to obtain a solid-liquid mixed product;

[0053] (4) Add 300ml ethylene dichloride to the three-necked flask, stir for 10min, then filter through a dry filter to obtain solid product and remaining mother liquor;

[0054] (5) After concentrating the remaining mother liquor, some solids wer...

Embodiment 2

[0063] The present invention relates to a kind of preparation method of penoxsulam, comprising the following steps:

[0064] A. Synthesis of intermediate products

[0065] (1) Dissolve 1mol trimethylchlorosilane and 1mol sodium iodide in a three-necked flask filled with 400ml of anhydrous acetonitrile, and stir evenly; the temperature during the feeding process is controlled at 0-40°C;

[0066] (2) At room temperature, stir 0.5mol 5,8-dimethoxy-[1,2,4]triazol[1,5-c]pyrimidin-2-amine and 0.5mol triethylamine in a beaker mix;

[0067] (3) Add the mixed triethylamine solution dropwise to the three-necked flask being stirred, and stir and react for 4 hours after the dropwise addition to obtain a solid-liquid mixed product;

[0068] (4) Add 300ml ethylene dichloride to the three-necked flask, stir for 10min, then filter through a dry filter to obtain solid product and remaining mother liquor;

[0069] (5) After concentrating the remaining mother liquor, some solids were precipit...

Embodiment 3

[0078] The present invention relates to a kind of preparation method of penoxsulam, comprising the following steps:

[0079] A. Synthesis of intermediate products

[0080] (1) Dissolve 0.6mol trimethylchlorosilane and 0.6mol sodium iodide in a three-necked flask filled with 400ml of anhydrous acetonitrile, and stir evenly; the temperature during the feeding process is controlled at 0-40°C;

[0081] (2) At room temperature, stir 0.5mol 5,8-dimethoxy-[1,2,4]triazol[1,5-c]pyrimidin-2-amine and 0.5mol triethylamine in a beaker mix;

[0082] (3) Add the mixed triethylamine solution dropwise to the three-necked flask being stirred, and stir and react for 4 hours after the dropwise addition to obtain a solid-liquid mixed product;

[0083] (4) Add 300ml ethylene dichloride to the three-necked flask, stir for 10min, then filter through a dry filter to obtain solid product and remaining mother liquor;

[0084] (5) After concentrating the remaining mother liquor, some solids were prec...

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Abstract

The invention relates to a method for synthesizing penoxsulam. The method comprises following steps: 1), 5,8-dimethoxy-[1,2,4]triazole[1,5-c]pyrimidine-2-amine is subjected to condensation with chlorosilane and sodium iodide under the action of nucleophilic alkali, and an intermediate is obtained; 2), the intermediate is subjected to a reaction with 2-(2,2-difluoroethoxy)-6-(trifluoromethyl)benzenesulfonyl chloride, and penoxsulam is produced. According to the method, by means of introduction of a tri-alkylated silicon derivative as the intermediate, the condensation reaction of an amino triazole group and a sulfonyl chloride group can be promoted, the reaction time is effectively shortened, reaction yield is increased, and product quality is improved. Besides, the method is green and environmentally friendly, is free of emission of reagents harmful to the environment and facilitates large-range popularization.

Description

technical field [0001] The invention belongs to the technical field of pesticide synthesis, and in particular relates to a preparation method of penoxsulam. Background technique [0002] Penoxsulam, chemical name: 2-(2,2-difluoroethoxy)-6-trifluoromethyl-N-(5,8-dimethoxy-[1,2,4] Triazolo[1,5-c]pyrimidin-2-yl)benzenesulfonamide, English name: Penoxsulam, CAS accession number: 219714-96-2, its structural formula is as follows: [0003] [0004] Penoxsulam is a triazolopyrimidine sulfonamide herbicide. It is a broad-spectrum herbicide for paddy fields. Barnyardgrass), an annual Cyperaceae weed, is effective against many broad-leaved weeds, and the effective period is as long as 30 to 60 days. One application can basically control the damage of weeds in the whole season, and it is very safe for rice. After years of marketing, this product has been enthusiastically sought after and favored by customers in the global market, and the market prospect is very broad. [0005] Fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
Inventor 戴百雄熊传宗张建广连建军卢威罗斌
Owner 湖北犇星农化有限责任公司
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