A kind of preparation method of herbicide saponin

A technology of saponin and phase transfer catalyst, which is applied in the field of preparation of herbicide saponin, which can solve the problems of cumbersome operation, poor product quality and production safety, simplify the operation process, avoid thermal decomposition, and reduce production costs Effect

Active Publication Date: 2011-11-30
SHENYANG SINOCHEM AGROCHEMICALS R&D CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of simple and convenient operation, safe and reliable, green environmental protection, high yield, good product quali

Method used

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  • A kind of preparation method of herbicide saponin
  • A kind of preparation method of herbicide saponin

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Under stirring, 124 g (0.5 mol) of 2-chloro-N-(4-chlorophenyl)-N-isopropylacetamide was added to 447 g of 22% (w / w, 0.5 mol) O, O- Add 1.0 g of triethylbenzyl ammonium chloride to the potassium dimethyl dithiophosphate aqueous solution, heat to 60° C., and keep the temperature for 3 hours. After the reaction, the temperature was slowly reduced to 5°C for about 2 hours, and the temperature was kept for 1 hour to make the product precipitate completely. Filter and wash the filter cake twice with 300 ml of water. Drying below 50°C yields 166.2 g of the target product Sabiphos, appearance: white solid, content: 94.6%, yield: 85.5%, melting point: 50-51°C.

Embodiment 2

[0024] Under stirring, 124 g (0.5 mole) of 2-chloro-N-(4-chlorophenyl)-N-isopropylacetamide was added to 497 g of 20% (0.55 mole) O, O-dimethyl bis Add 0.6 g of tetrabutylammonium chloride to the sodium thiophosphate aqueous solution, heat the temperature to 50°C, and keep the temperature for 5 hours. After the reaction, the post-treatment steps are the same as in Example 1. Obtained 169.8 grams of sabarnyl phosphorus, appearance: white solid, content: 96.1%, yield: 88.7%, melting point: 50-51°C.

Embodiment 3

[0026] Under stirring, 124 g (0.5 mole) of 2-chloro-N-(4-chlorophenyl)-N-isopropylacetamide was added to 100 g (0.55 mole) of O,O-dimethyl dithiophosphoric acid Add 0.2 g of tetrabutyl ammonium chloride to the solution formed by ammonium and 200 ml of water, heat the solution to 50° C., and keep the temperature for 5 hours. According to high performance liquid chromatography analysis, when the content of 2-chloro-N-(4-chlorophenyl)-N-isopropylacetamide is less than 0.5%, the reaction ends. After the reaction, the post-treatment steps are the same as in Example 1. Obtained 167.4 grams of sabarnyl phosphorus, appearance: white solid, content: 94.3%, yield: 85.8%, melting point: 50-51°C.

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Abstract

The invention discloses a preparation method of herbicide anilofos with water as a solvent. A proper amount of a phase transfer catalyst is added during a reaction procedure; condensation and crystallization are completed in a single step; when the reaction is finished, a reaction liquid is cooled; anilofos crystals are directly precipitated in water; the crystals are filtered and washed, such that anilofos products are obtained. According to the invention, no organic solvent or heat precipitation procedure is adopted during the reaction procedure. Therefore, a potential danger that the product is easy to be decomposed under heat is avoided from the source, and product yield and quality are improved. The preparation method of herbicide anilofos provided by the invention has advantages of easy operation, environment protection, high product yield and good product quality. The method is green, safe, reliable, and is suitable for industrialized productions.

Description

Technical field [0001] The invention belongs to the field of organic synthesis, and specifically relates to a preparation method of the herbicide saraphos. technical background [0002] The chemical name of sarcophos (English common name anilofos) is: O,O-dimethyl-S-4-chloro-N-isopropylphenylcarbamoyl methyl dithiophosphate, which is a phosphorothioate Ester herbicides are mainly used in paddy fields to control annual gramineous and Cyperaceae weeds. The structural formula of Sabiphos is: [0003] [0004] Patent BR7804448, DE2604225 and Pesticides. 1989, 28(3), 7 and other documents reported the synthesis method of sarcophos. The reaction equation is as follows: [0005] [0006] The preparation method of saraphos reported in the above literature is: dissolving 2-chloro-N-(4-chlorophenyl)-N-isopropylacetamide (compound II) in an organic solvent, and then adding O, O- Dimethyl dithiophosphoric acid (compound III, X=H, hereinafter referred to as methyl sulfide) react with acid bind...

Claims

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Application Information

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IPC IPC(8): C07F9/165
Inventor 薛有仁叶艳明侯广新于春睿于福强刘春成崔广坚
Owner SHENYANG SINOCHEM AGROCHEMICALS R&D CO LTD
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