- Preparation method of glufosinate-ammonium
-
The invention discloses a preparation method of glufosinate-ammonium. The preparation method comprises the following steps that 1, in alkaline environment, 4-(hydroxymethyl phosphono)-2-carbonyl butyric acid (I) and a benzylamine solution react to produce 2-[( phenyl amino)-4-(methyl sodium phosphate)-sodium butyrate (II); 2, 2-[(phenyl amino)-4-(methyl sodium phosphate)-sodium butyrate (II) is subjected to acid hydrolysis to obtain glufosinate-ammonium (III). Compared with the prior art, the preparation method has the advantages that the conditions are mild; the yield of the glufosinate-ammonium is high; the purity is high.
- -
-
Paragraph 0034;0037-0038; 0042-0044; 0047-0048
(2020/06/30)
-
- Process for preparing glufosinate acid with hydrogenation method
-
The invention discloses a process for preparing precursor glufosinate acid of glufosinate acid with a catalytic hydrogenation method. The process comprises the following steps: firstly, reacting N-ethyl acetamidomalonate with 2-[ethyoxyl(methyl)phosphonyl] acetaldehyde under the actions of an acid binding agent and a dehydrating agent to generate an intermediate, namely, 2-acetamido-4-[ethyoxyl(methyl)phosphonyl]butyl-2-olefine acid ester; secondly, separating and purifying the intermediate, performing hydrogenation by taking ethanol as a solvent under the catalytic action of a hydrogenation catalyst to obtain a product, namely, 2-acetamido-4-[ethyoxyl(methyl)phosphonyl]ethyl butyrate, wherein the two-step yield can be 85 percent or more; lastly, performing deprotection with concentrated hydrochloric acid, and removing the hydrochloric acid to obtain the glufosinate acid. The process has the advantages of easiness in reaction and post-treatment operation, high yield, recyclability of the hydrogenation catalyst and the like, and has a very wide industrial prospect.
- -
-
Paragraph 0012; 0029
(2018/07/30)
-
- Glufosinate ammonium preparation method
-
The invention relates to a glufosinate ammonium preparation method. According to the present invention, nitro is introduced by using a simple and economical method, and is reduced under a mild condition so as to introduce amino group as the key step, such that the method for introducing amino by using other expensive amino acid derivatives or other toxic nitrogen-containing compounds is avoided, and the amino protection and deprotection during the reaction is eliminated; and the preparation method has advantages of simple reaction process, mild condition, simple and easily-available raw materials, simple operation and good atom economy, and is extremely suitable for industrial production.
- -
-
Paragraph 0028; 0032
(2018/07/07)
-
- A aminonitrile preparation method and process for the preparation of the intermediates of glufosinate
-
The invention discloses a preparation method of amino-nitrile and an intermediate for preparing glufosinate-ammonium. The preparation method disclosed by the invention aims at solving the problem of low glufosinate-ammonium yield by using acetal in the existing methods. Different from the existing methods for preparing glufosinate-ammonium, the method disclosed by the invention comprises the following steps: firstly reacting acetal with acetylchloride to obtain an enol ether intermediate, reacting the enol ether intermediate with sodium cyanide to obtain amino-nitrile, and finally hydrolyzing the amino-nitrile to obtain the glufosinate-ammonium. The method has the advantages of higher reaction yield and capacity of remarkably reducing the production cost of the glufosinate-ammonium.
- -
-
Paragraph 0037; 0042-004
(2017/08/25)
-
- LJ reaction in the preparation wittich reagent and application of glufosinate in
-
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.
- -
-
Paragraph 0099; 0101
(2017/12/04)
-
- NOXIOUS ARTHROPOD CONTROL AGENT CONTAINING AMIDE COMPOUND
-
An object of the present invention is to provide a compound having the controlling activity on a noxious arthropod, and a noxious arthropod controlling agent containing an amide compound of formula (I): wherein X represents a nitrogen atom or a CH group, p represents 0 or 1, A represents a tetrahydrofuranyl group or the like, R1, R2, R3, R4, R5, R6 and R7 represent a hydrogen atom or the like, n represents 1 or 2, Y represents an oxygen atom or the like, m represents any integer of 0 to 7, and Q represents a C1-8 chain hydrocarbon group optionally having a phenyl group or the like, has the excellent noxious arthropod controlling effect.
- -
-
-
- Grass ammonium phosphine method for the preparation of
-
The invention belongs to the field of chemical synthesis, and particularly relates to a new preparation method of a glufosinate-ammonium weed killer. The preparation method is characterized in that methyl phosphorus dichloride reacts with alcohol so as to prepare a methyl phosphonate compound IV, and then the methyl phosphonate compound IV reacts with acrolein so as to prepare a methyl propionaldehyde phosphonate compound II; the methyl propionaldehyde phosphonate compound II is subjected to Bucherer-Bergs ring-closure reaction so as to prepare a hydantoin derivative shown in a formula III, and the hydantoin derivative is subjected to hydrolysis reaction so as to prepare the glufosinate-ammonium compound shown in a formula I. The preparation method of the glufosinate-ammonium has the advantages that required conditions are mild, the detection is easy, the required raw materials are easily available and low in cost, the yield of the obtained product is high, the obtained product has high purity, and ammonium salt is removed without needing recrystallization over and over again.
- -
-
Paragraph 0067; 0069; 0070
(2017/01/17)
-
- Grass amine phosphine method for the preparation of
-
The invention discloses a Glufosinate-ammonium and its derivative improved preparation method, the method comprises the following steps: diethyl methyl-phoshphonite, acraldehyde and acetic anhydride are subjected to an addition reaction, a reactant, sodium cyanide (editpotassium cyanide for replacing) and an ammonia water solution of ammonium chloride are subjected to an improved STRECKER reaction without separation, the product is subjected to hydrolysis and ammonification for forming salt to obtain Glufosinate-ammonium. The preparation method has the characteristics of high selectivity and high yield.
- -
-
Sheet 0018; 0022; 0035; 0040; 0041; 0042; 0043
(2017/04/28)
-
- A kind of preparation method for treating keratoconjunctival and wherein the intermediate preparation method
-
The invention relates to the technical field of pesticides and particularly relates to a method for preparing glufosinate-ammonium and a preparation method for an intermediate thereof. The method is characterized by comprising the following steps of: taking phosphorus trichloride and phosphite ester as raw materials, preparing chlorophosphite ester under the catalysis of the mixture of triethylamine, N,N-dimethylformamide or pyridine and hexamethylphosphoramide, preparing methylmagnesium chloride from chloromethane and magnesium metal, preparing methyl phosphite ester by reacting the chlorophosphite ester with methylmagnesium chloride, carrying out an addition reaction on the methyl phosphite ester and acrolein, carrying out a Strecker reaction on the product of the addition reaction, sodium cyanide, ammonium chloride and ammonia water under the catalysis of montmorillonite-supported lewis acid, and carrying out hydrolyzing and purifying after finishing the Strecker reaction, so as to obtain the high-purity glufosinate-ammonium. The method provided by the invention has the advantages that side reactions are few, products are high in purity and easy to separate, and catalysts and solvents are easy to obtain, regenerate and recycle; and the production cost is lowered, and the method is accordant with the trend of green chemical industry and is suitable for industrial production.
- -
-
Paragraph 0119; 0120
(2017/03/08)
-
- Purification method of glufosinate
-
The invention relates to a purification method of glufosinate. The method comprises the following steps: adding a glufosinate hydrochloride crude product into a solvent, adding amino acid and an aqueous solution of alkali, reacting for 0.5-1.5 h, adjusting pH of the reaction system to 1-7, filtering and drying to obtain glufosinate-ammonium acid; and dissolving glufosinate-ammonium acid in a solvent, introducing ammonia gas and carrying out a salt-forming reaction, precipitating a glufosinate solid, filtering and drying to obtain high-purity glufosinate. According to the purification technology, use of fatty amine which is hard to remove and high-risk oxirane and epoxypropane is avoided. The steps are simple. The obtained glufosinate has low content of inorganic salt, high purity, high yield and high safety. In addition, water or alcohol is used as a solvent in the technological process, and a neutralization reaction is carried out by the use of ammonia water and inorganic base. The purification method accords with the ecology and economy principle, and has a good industrial prospect. In addition, purification is carried out by addition of amino acid, and purification efficiency and product purity are higher.
- -
-
Paragraph 0027
(2016/11/02)
-
- The purification process of a grass ammonium phosphine
-
The invention provides a glufosinate purifying technology including the following steps: (1) adding glufosinate hydrochloride to alcohol R1OH, adding R2NH2 for ammoniation, adjusting the pH to 7.0-14.0, cooling and filtering, removing a solvent from a filtrate to obtain glufosinate ammonium salt and a small amount of organic impurities; (2) dissolving the glufosinate ammonium salt obtained by the steps (1) in an appropriate amount of water, leading in CO2 for neutralizing to the pH of 2.0-5.0, adding a proper amount of alcohol R3OH for precipitation of glufosinate acid, centrifugally filtrating to obtain the glufosinate acid which contains a small amount of ammonium hydrogen carbonate or organic amine carbonates; (3) heating for drying a glufosinate acid filtering cake obtained by the step (2) for decomposition and volatilization of the ammonium hydrogen carbonate or organic amine carbonates to obtain high purity glufosinate acid. The glufosinate purifying technology is simple in steps, the obtained glufosinate is low in inorganic salt content and high in purity, and compared with a traditional technology using epoxy ethane and epoxy propane, the purifying technology using carbon dioxide for separation of glufosinate hydrochloride and HCl is more economical, and high in safety, and has a higher industrialization prospect.
- -
-
Paragraph 0022-0028
(2016/10/10)
-
- Method for preparing high-purity glufosinate-ammonium by organic alkali process
-
The invention discloses a method for preparing high-purity glufosinate-ammonium by an organic alkali process. The method comprises the following steps: by using a glufosinate-ammonium hydrochloride solution as a raw material, filtering the raw material, concentrating, directly adding tertiary amine R1R2R3N1 into the concentrated solution under the heating condition of 60-80 DEG C, and keeping the temperature to carry out hydrochloric acid removal reaction; after the reaction finishes, cooling to -3 to -8 DEG C to precipitate a glufosinate-ammonium free acid crude product; adding alcohol into the crude product, pulping, and filtering, wherein the obtained filter cake is glufosinate-ammonium free acid; adding alcohol into the glufosinate-ammonium free acid, heating to 30-50 DEG C, introducing ammonia gas to react; and after the reaction finishes, cooling to crystallize, filtering, and drying to obtain the glufosinate-ammonium with the purity of at least 88%.
- -
-
Paragraph 0045
(2016/10/20)
-
- Purification method for glufosinate-ammonium
-
The invention relates to a purification method for glufosinate-ammonium. The method comprises the following steps that a glufosinate-ammonium hydrochloride crude product is dissolved into a solvent, then, alkaline is added to be subjected to a reaction, the pH value is adjusted to be 7-10, reduced pressure distillation is performed to remove some solvent, then filtering is performed to remove ammonium chloride and other undissolved substances; acid is added into the reaction solution to be subjected to a reaction, the pH value is adjusted to be 1-4.5, and then filtering and drying are performed to obtain glufosinate-ammonium acid; the glufosinate-ammonium acid is dissolved into the solvent, then, ammonia gas is introduced to be subjected to a salt forming reaction, glufosinate-ammonium solid is separated out, and filtering and drying are performed to obtain high-purity glufosinate-ammonium. According to the purification technology, fatty amine hard to remove and high-risk ethylene oxide and epoxypropane are prevented from being used, the steps are simple, the obtained glufosinate-ammonium is low in inorganic salt content and high in purity, yield and safety, water or alcohol is used as the solvent in the technological process, ammonium hydroxide and inorganic base are used for being subjected to a neutral reaction, the glufosinate-ammonium conforms to the environment-friendly and economical principle, and the good industrial prospect is achieved.
- -
-
Paragraph 0026
(2017/02/09)
-
- A glufosinate hydrochloride by the method of preparation grass ammonium phosphine acid (by machine translation)
-
The present invention discloses a one-glufosinate hydrochloride by the method of preparation grass ammonium phosphine acid, firstly the glufosinate hydrochloric acid salt is dissolved in the alcohol, then adding ammonia in and after the, precipitated grass ammonium phosphine acid. The method of the invention not only can be obtained in high yield high-purity grass ammonium phosphine acid, but also can save a large amount of water and alcohol, is suitable for industrial application. (by machine translation)
- -
-
Paragraph 0023-0032; 0033; 0034
(2017/05/16)
-
- Method of manufacturing a dry water-soluble herbicidal salt composition
-
A method of manufacturing a solid, water-soluble herbicidal composition comprising a water-soluble salt of a herbicidal compound is disclosed. The herbicidal compound is a water-insoluble compound that includes a carboxylic acid functionality, such as a phenoxy-substituted carboxylic acid compound or a substituted benzoic acid compound, and is sufficiently pure to form a dry, solid herbicidal salt composition after interaction with a suitable neutralizing base, such as ammonia, an alkylamine, a dialkylamine, a trialkylamine, a hydroxyalkylamine, a dihydroxyalkylamine, an alkaline salt of an alkali metal or a combination thereof. The dry herbicidal salt composition includes at least about 90% by weight of the water-soluble herbicidal salt, and dissolves rapidly and essentially completely in water to form an aqueous herbicidal solution including up to about 75% by weight of the water-soluble herbicidal salt.
- -
-
-
- 4-phosphorus-2-phthalimidobutyrate intermediates
-
Phosphinylbutanoic acids, such as phosphinothricin, can be prepared by reacting racemic 4-halo-2-phthalimidobutyrates with a tricoordinate phosphorus compound represented by the formula: wherein R1 is methyl or ethyl, and R2 is selected from the group consisting of alkoxy having from one to six carbon atoms, aryloxy, and trialkylsilyloxy groups having from one to twelve carbon atoms, to form an intermediate compound; and hydrolyzing the intermediate compound to form the phosphinylbutanoic acids.
- -
-
-
- Phenoxycarboxylic acid compounds and herbicide comprising it as active ingredient
-
A novel phenoxycarboxylic acid of formula (I) is disclosed. The compound is effective as herbicide for eradicating broad-leaved weeds. A combination of the phenoxylcarboxylic acid and a N-phosphonomethylglycine or a glufosinate which is known as a herbicide is very effective for eradicating both broad-leaved weeds and narrow-leaved weeds.
- -
-
-
- Asymmetric Synthesis of (+)-Phosphinothricin and Related Compounds by the Michael Addition of Glycine Schiff Bases to Vinyl Compounds
-
(S)-(+)-Phosphinothricin was prepared in good optical yield by th Michael addition of chiral glycine Schiff base derived from (S)-2-hydroxy-3-pinanone to vinyl phosphorus compound. (R)-(-)-Phosphinothricin, an enantiomeric isomer, can also be prepared from the same chiral glycine Schiff base by choosing suitable reaction temperature.
- Minowa, Nobuto,Hirayama, Masao,Fukatsu, Shunzo
-
p. 1761 - 1766
(2007/10/02)
-
- FACILE SYNTHESIS OF D,L-PHOSPHINOTHRICIN FROM METHYL 4-BROMO-2-PHTHALIMIDOBUTYRATE
-
Synthetic versatility of the title bromide is illustrated by simple preparations of D,L-phosphinothricin, D,L-2-amino-4-phosphonobutyric acid, and aminocyclopropanecarboxylic acid.
- Logusch, E. W.
-
p. 5935 - 5938
(2007/10/02)
-
- Process for preparing optically active [(3-amino-3-carboxy)propyl-1]_phosphinic acid derivatives
-
Disclosed is a novel process for optically active [(3-amino-3-carboxy)propyl-1]phosphinic acid derivatives, which comprises reacting a Shiff's base with a derivative of vinylphosphinate in the presence of a base, and subjecting the resulting compound to hydrolysis to form the optically active [(3-amino-3-carboxy)propyl-1]phosphinic acid derivatives as either [L-(3-amino-3-carboxy)propyl-1]phosphinic acid derivatives or [D-(3-amino-3-carboxy)propyl-1]phosphinic acid derivatives.
- -
-
-
- Phosphorus-containing compounds and process for producing the same
-
2-Amino-4-(hydroxy)phosphinoylbutyryl-L-alanyl-L-alanine.
- -
-
-
- A PRACTICAL SYNTHESIS OF (+/-)-PHOSPHINOTHRICINE
-
A practical synthesis of (+/-)-phosphinothricine from trimethyl phosphite is described.
- Minowa, Nobuto,Fukatu, Shunzo,Niida, Taro,Takada, Masao,Sato, Kikumasa
-
p. 2391 - 2392
(2007/10/02)
-
- Herbicidal agents
-
Herbicidal agents, containing as active ingredient a compound of the formula STR1 or their salts with acids, are useful for combatting a great variety of mono- and dicotyledonous weeds. In the formula R1 is methyl or halomethyl, R2 is OH, SH, OM or SM (M=equivalent of a base), R3 is the same as R2 or an ester, amide or hydrazide group, R4 and R5 are preferably hydrogen and X is oxygen or sulfur.
- -
-
-
