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Isomerization reaction

A technology of isomerization reaction and reaction, which is applied in application, biocide, plant growth regulator, etc., can solve the problem of high cost of wastewater treatment

Inactive Publication Date: 2012-02-01
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Pesticides such as acephate, glyphosate, and glufosinate have already achieved a total annual sales of more than 20 billion U.S. dollars in the international market, and are still expanding at an average annual rate of 5%. However, to produce one ton of these products now, A large amount of waste water is bound to be associated. So far, according to the traditional organic phosphorus reaction methods and technologies, the problem of such a large amount of waste water associated with these products cannot be solved, especially the existing glyphosate production is accompanied by a large amount of high-content sodium chloride waste water. The waste water cannot be treated by conventional methods, so the cost of waste water treatment is very high. There are more than 500 production enterprises in my country alone, and the pressure on environmental protection is very serious. Only the source of the process can solve the waste water problem, that is, create a new clean production The process route can fundamentally solve the problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0124] Throw 100 grams of 98% phosphorous trichloride and 100 grams of anhydrous n-hexane into a four-necked reaction bottle, start stirring, heat up to reflux, add 28-37 g of anhydrous methanol dropwise, HCl gas continuously overflows, and reflux reaction for 16 After ~30 hours, when the HCl gas basically does not overflow, it is the end of the reaction. Cool down to normal temperature, let stand for more than 7 hours, divide into two layers, and separate the lower layer, which is the intermediate 10 compound. The average yield is 90 grams, the content is 98%,

[0125] Use n-hexane (or N, N-dimethylformamide) to prepare a 10-20% solution of compound 10, put it into a reaction bottle, control the temperature from 40°C to reflux, slowly and evenly add 34 grams of 99% acetamide solid, Constantly have HCl gas to overflow, react after 14 hours, basically do not have HCl gas to overflow and be the reaction end point, cool down to normal temperature, leave standstill for 7 hours, a ...

Embodiment 2

[0127] Throw 250 grams of anhydrous trimethyl phosphate (or N,N-dimethylformamide) into the reaction bottle, start stirring, control the temperature at 20-40°C, slowly add 50 grams of 98% glycine hydrochloride, and dissolve all After the solution becomes clear, slowly add 13 grams of paraformaldehyde, stir the reaction at this temperature until the solution is clear and transparent, cool down to about 15°C, add 61 grams of 98% phosphorus trichloride dropwise, , under the protection of isolated air or nitrogen, stirred and reacted for 14-20 hours, a large amount of solids precipitated, filtered and dried at room temperature and under the condition of isolated air to obtain 88 g of compound 11, with a content of 98%; the mother liquor was applied mechanically;

[0128] Put 88 grams of compound 11 into the reaction bottle, start stirring, slowly add 250 grams of 50-70% methanol aqueous solution, control the temperature at 40°C to reflux, react for 2-8 hours, then distill, and when...

Embodiment 3

[0130] 0.03mol of La(NO 3 ) 3 ·6H 2 O and GdCl 3 ·6H 2 O catalyst was added to 1mol of 3-hydroxypropionaldehyde and 1mol of NaCN in aqueous solution, stirred at room temperature for 15 minutes and all dissolved, then slowly added 1mol of formamide (or acetamide or saturated methanol / ammonia solution) and reacted at 40°C After 3 hours, the reaction solution was concentrated, and the residue was separated through a silica gel column (cycloethane-ethyl acetate) to obtain 104 g of compound 12 liquid, with a content of 98%;

[0131] This 104 grams of compound 12 is dropped into excess (300 grams) of phosphorus trichloride, or dropped into an equimolar compound of 9, the temperature is controlled below 20°C, the reaction is stirred, and the liquid chromatography normalization method is used to test the reaction system When the content of compound 12 is less than 1%, it is the end of the reaction, a large amount of solids are precipitated, filtered, and dried to obtain an average...

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Abstract

The invention discloses a highly selective novel reaction with an important application value in organic phosphorus synthesis methodology. The reaction can be applied in important pesticide commodities of acephate, glyphosate, glufosinate-ammonium, chloramine phosphorus, profenofos, and the like. With the reaction, innovative technical synthetic routes can be designed. With the reaction, standards of clean production technologies can be satisfied, and the production cost is greatly reduced compared to existing technical routes.

Description

[0001] The present invention relates to a new high-selectivity reaction with great application value in the synthetic methodology of organophosphorus, which is applied to important compounds such as acephate, glyphosate, glufosinate-ammonium, chloramidophos, and profenofos For pesticide commodities, an innovative process synthesis route has been designed, which not only meets the standard of clean production process, but also greatly reduces the preparation cost compared with the existing process route. Background technique [0002] Organophosphorus chemistry is one of the four main pillars of current elemental organic chemistry. Organophosphorus compounds have important applications in pesticides, medicines, extractants, flame retardants, etc., as well as in organic synthetic chemistry. The research of compounds is also of great significance in life science research. Phosphorus (phosphonate) esters and thiophosphorus (phosphonic) ester derivatives are the most studied compounds...

Claims

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Application Information

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IPC IPC(8): C07F9/42C07F9/50C01B25/163C01B25/10C07C255/26C07F9/6584C07F9/34C07F9/6561C07F9/58C07F9/17C07F9/20C07F9/38C07F9/18C07F9/24A01N57/20A01N57/16A01N57/14A01P7/00
Inventor 李坚
Owner WUHAN INSTITUTE OF TECHNOLOGY
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