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Application of LJ reaction in preparation of wittig reagent and glufosinate-ammonium

A glufosinate-ammonium reaction technology, applied in the application field of LJ reaction in the preparation of Wittig reagent and glufosinate-ammonium, can solve the problems of only 4% utilization rate, non-compliance, inconvenient product separation and purification, etc.

Active Publication Date: 2012-03-14
PAPANNA BEIJING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, from the point of view of modern industrialization implementation, Wittig reaction also has two main shortcomings: (1) after the reaction finishes, the phosphorus oxide by-product that produces can be dissolved in organic solvent and cause the separation and purification of product to be inconvenient ; (2) Although the Wittig reaction yield is high, its atom utilization is very low, which does not meet the principles of modern clean production processes, for example, in the Wittig reaction participated by bromide methyltriphenylphosphine molecules , only the methylene group is utilized in the product, only 14 parts of the 356 parts of the mass of the reagent molecule are used, the utilization rate is only 4%, and 278 parts of the "waste" triphenylphosphine oxide are produced

Method used

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  • Application of LJ reaction in preparation of wittig reagent and glufosinate-ammonium

Examples

Experimental program
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Effect test

Embodiment 1

[0088] Molecular ratio phosphorus trichloride: methyl chloride = 1:1

[0089] Throw 100 grams of 98% phosphorus trichloride into the pressure reactor, under the condition of isolating air and water, control 20-110 ℃, add the calculated amount of methyl chloride / chloroform saturated solution dropwise, keep warm for 2 hours, steam Remove the chloroform solvent, let it stand, crystallize, filter, dry, and obtain quarter Salt 6 is solid, the yield is 98%, and the content is 98%.

[0090] Because 6 is unstable in air and water, dissolve it in dichloroethane, control the temperature below 20°C, slowly add equal mol of aluminum trichloride, keep warm for 4 to 8 hours, then add dichloride dichloride dropwise. Phosphorus, a large amount of precipitates were precipitated, filtered, and the mother liquor was vacuum distilled, and the distillation substrate was 8 compounds, with a yield of 98% and a content of 98%.

Embodiment 2

[0092] Throw 100 grams of 98% phosphorus trichloride into the reaction bottle, under the condition of isolating air and water, control the temperature below 54°C, add dropwise a calculated amount of 20-40% trimethyl chloride phosphate solution, and generate in one step Simultaneously with compound 8, hydrogen chloride was produced. After reacting for 4 to 8 hours, a large amount of solids precipitated out. After standing still, crystallized, filtered, and dried in vacuo, compound 8 was obtained with a yield of 98% and a content of 98%.

Embodiment 3

[0094] Prepare a 10-20% solution of 8 prepared in Example 2 and trimethyl phosphate, put it into a reaction flask, control the temperature below 5°C, add benzophenone in equal moles dropwise, and react for 2 hours to generate 1,1- Stilbene and phosphorus oxychloride, the yield is 85%.

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Abstract

The present invention relates to an application of a new LJ intramolecular isomerization reaction in preparation of a wittig reagent and a herbicide of glufosinate-ammonium. With the application, a new approach of a synthesis route for preparing the wittig reagent and the glufosinate-ammonium is developed, the disadvantages of the existing wittig reaction are improved, and the industrial design of the glufosinate-ammonium production is improved.

Description

[0001] The present invention relates to a new reaction of intramolecular isomerization of LJ, and its application in Wittig phosphine reagent and herbicide glufosinate-ammonium. The shortcomings of the original Wittig reaction have improved the industrial design of glufosinate-ammonium production. Background technique [0002] On July 18, 2010, the applicant for the patent of this invention applied for an invention patent with the application number 201010237200.0 and the name "LJ isomerization reaction". A patent application fills it up. The Wittig reaction is one of the most important reactions used to form carbon-carbon double bonds in organic chemistry. The reaction is named after Georg Wittig, a German organic chemist who made outstanding contributions to the reaction. Chemist H.C. Brown shared the 1979 Nobel Prize in Chemistry for his development of phosphorus compounds as important reagents in organic synthesis. This discovery can be widely used in the synthesis of pha...

Claims

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Application Information

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IPC IPC(8): C07F9/28C07F9/32C07F9/52C07F9/42C07F9/30C07F9/38C07F9/535C07F9/34C07C255/30C07C21/08C07C1/34
Inventor 李坚
Owner PAPANNA BEIJING TECH
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