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Synthesis method of glufosinate-ammonium intermediate

A synthesis method and intermediate technology, which are applied in the synthesis field of glufosinate-ammonium intermediates, can solve the problems of unsuitability for industrial production, high price, poor atom economy and the like, and achieve the advantages of avoiding the generation of mixed salts, easy operation and short reaction period. Effect

Active Publication Date: 2019-12-20
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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Problems solved by technology

[0003] Glufosinate-ammonium cyanide is an important intermediate in the synthesis process of glufosinate-ammonium. The intermediate grass is obtained by the addition reaction of methyl phosphite and acrolein, acidolysis, and reaction with cyanide and ammonia / ammonium chloride. Ammonium phosphine cyanide, traditional cyanide is sodium cyanide, potassium cyanide, therefore will face the separation problem of ammonium chloride and sodium chloride or potassium chloride, CN109879910A invented with trimethylsilyl cyanide as cyanide reagent, However, it is expensive and has poor atom economy, so it is not suitable for industrial production
[0004] At present, there is no report yet to use ammonium cyanide as a cyanide reagent for the synthesis of glufosinate-ammonium intermediate cyanamide

Method used

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  • Synthesis method of glufosinate-ammonium intermediate

Examples

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Embodiment 1

[0027] The synthesis steps of ammonium cyanide aqueous solution are: dissolve 45g of sodium cyanide in 100g of water, add 73g of ammonium bicarbonate in batches, stir at 10-20°C for 1 hour after the addition, and filter out sodium bicarbonate to obtain ammonium cyanide Aqueous solution, wherein the mass content of ammonium cyanide is about 27%.

Embodiment 2

[0029] Add 150ml of ethanol and diethyl methylphosphite (68g, 0.5mol) in turn to the reaction flask, under the protection of nitrogen, add acrolein (28g, 0.5mol) dropwise at 15°C, and control the dropping time to 2h, After the dropwise addition, react at 25°C for 2 to 3 hours. After the reaction, distill under reduced pressure to obtain the residue 3-(methylethoxy)phosphoryl propionyl diethyl alcohol. Add 50g of 5% hydrochloric acid dropwise to the residue at 15°C, and control the dropping time for 2h. After the dropwise addition, keep the temperature at 20°C for 2h, and distill under reduced pressure after the reaction to obtain 78g of ethyl methylpropionyl phosphate , content 97.9%, yield 93.1%.

Embodiment 3

[0031] Add 27% ammonium cyanide aqueous solution (wherein containing ammonium cyanide 5.26g, 119.4mmol), ammonium chloride (6.45g, 119.4mmol) and 20% ammoniacal liquor 10g (wherein NH 3 119.4mmol), at 10°C, dropwise added ethyl methylpropionyl phosphate (10g, 59.7mmol) prepared in Example 2, after the dropwise addition, the temperature was raised to 30°C, reacted for 2 hours, and added 45g of 30% For industrial hydrochloric acid, the temperature was raised to reflux for 1 hour, the temperature was lowered to cool, ammonia was passed through, the ammonium chloride was filtered out, and methanol was added to crystallize to obtain 11.6 g of white glufosinate-ammonium aminonitrile solid with a content of 97% and a yield of 99.2%.

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Abstract

The invention relates to a synthesis method of a glufosinate-ammonium intermediate. The synthesis method comprises the following step: enabling ethyl methyl(3-oxopropyl)phosphinate and NH4CN to reactin the presence of ammonium chloride and ammonium hydroxide so as to obtain the glufosinate-ammonium intermediate, namely glufosinate-ammonium amino-nitrile (ethyl (3-amino-3-cyanopropyl)(methyl)phosphinate). By adopting the method provided by the invention, the situation that in a conventional process, a mixed salt of ammonium chloride and sodium chloride is generated can be effectively avoided,the problem of treating the mixed salt is solved from sources, trimethylsilyl cyanide which is high in price is not used as a cyaniding reagent, and in addition, the method provided by the invention has the characteristics of being mild in reaction condition and high in yield, so that the production cost can be lowered, and good industrial prospects can be achieved.

Description

technical field [0001] The invention specifically relates to a synthetic method of a glufosinate-ammonium intermediate. Background technique [0002] Glufosinate-ammonium ammonium salt, the chemical name is 4-[hydroxyl (methyl)phosphono]-DL-homoalanine, which was developed and produced by the German Hearst Company in the 1980s. In addition to herbicidal activity, It also has the characteristics of high efficiency, low toxicity and easy degradation. [0003] Glufosinate-ammonium cyanide is an important intermediate in the synthesis process of glufosinate-ammonium. The intermediate grass is obtained by the addition reaction of methyl phosphite and acrolein, acidolysis, and reaction with cyanide and ammonia / ammonium chloride. Ammonium phosphine cyanide, traditional cyanide is sodium cyanide, potassium cyanide, therefore will face the separation problem of ammonium chloride and sodium chloride or potassium chloride, CN109879910A invented with trimethylsilyl cyanide as cyanide r...

Claims

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Application Information

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IPC IPC(8): C07F9/32
CPCC07F9/3211
Inventor 姜宇华陈佳陶亚春栾小兵纪雷
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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