15715-41-0Relevant articles and documents
Synthesis method and synthesis device of diethyl methylphosphite
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Paragraph 0071-0118, (2020/09/09)
The invention relates to a synthesis method and a synthesis device of diethyl methylphosphite. The synthesis method comprises the following steps: (1) mixing methyl phosphine dichloride, absolute ethyl alcohol and a solvent to carry out a synthesis reaction; (2) carrying out reduced pressure deacidification treatment on the reaction solution obtained in the step (1); and (3) separating and purifying the deacidified reaction solution obtained in the step (2) to obtain diethyl methylphosphite. According to the synthesis method, an acid-binding agent is not needed, hydrogen chloride gas generatedby the synthesis reaction can be discharged through reduced-pressure deacidification treatment, the generation of solid waste residues containing acid-binding agent hydrochloride is avoided, the separation and treatment of the solid waste residues are reduced, and the dosage of ethanol is reduced by adding a solvent, so that the ethanol does not need to play a role as a solvent, the energy consumption is reduced, the resources are saved, the process is high in yield, simple to operate and environment-friendly, and the atom economy is good.
Purification method of dialkyl methylphosphite
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Paragraph 0041-0043; 0047-0052; 0059-0067; 0074-0083, (2020/12/15)
The invention relates to the technical field of compound purification, and particularly provides a purification method of dialkyl methylphosphite. The purification method comprises the following steps: adding a weak polar solvent into a reaction solution containing dialkyl methylphosphite, magnesium chloride and an ether solvent, conducting cooling to -10 DEG C to 40 DEG C, adding a nitrogen-containing organic alkali compound, carrying out a heat preservation reaction, and conducting filtering to obtain magnesium chloride and a filtrate; and rectifying the filtrate to obtain a dialkyl methylphosphite product. According to the purification method provided by the invention, the purity and the yield of the dialkyl methylphosphite are improved, the obtained magnesium chloride does not containcrystal water, the nitrogen content in the magnesium chloride is 0.01-0.5%, and the purity of the anhydrous magnesium chloride can reach 97% or above; and the purity of the obtained dialkyl methylphosphite product can reach 97% or above, and the yield can reach 85% or above. The method has the advantages of simple process, no need of special equipment, mild reaction conditions and no need of high-temperature distillation or low-temperature brine treatment process, and is suitable for large-scale industrial production.
A method for preparing methyl asia phosphine acid diethyl ester (by machine translation)
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Paragraph 0028-0032, (2019/07/06)
The invention discloses a method for preparing methyl asia phosphine acid diethyl ester, aims to solve the problems in the existing method, when using ammonia gas as acid, pH value of the reaction solution in the need to control the 7.0 - 8.5 between, accurate control of the pH value is very difficult, and is lower than the pH value, will produce a large number of methyl inferior phosphine acid ethyl ester by-product, the use of the organic amine do capture, there is caused a large toxicity, high price, the recovery process is tedious, the recovery rate is low. The present invention relates to methyl-phosphine, ethanol and calcium oxide as the main raw material, process for preparing methyl asia phosphine acid diethyl ester is obtained, which is a low-cost, is suitable for the industrial production of methyl asia phosphine acid diethyl ester preparation method. The invention in the preparation of the methyl asia phosphine acid diethyl ester, for the first time the adoption of the calcium oxide to replace the ammonia or organic amine as capture, effectively reduces the production cost, and the calcium oxide is non-toxic, is friendly to the environment, and has a good economic value and social value. (by machine translation)
A method for preparing methyl asia phosphine acid diethyl ester
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Paragraph 0036; 0037; 0038; 0039-0045, (2019/05/04)
The invention provides a method for synthesizing diethyl methyl-phosphonite. The method comprises technological steps as follows: firstly, a ternary complex is prepared from phosphorus trichloride, aluminium trichloride and chloromethane as raw materials, the ternary complex is reduced by powdered aluminium and reacts with absolute ethyl alcohol, a crude diethyl methyl-phosphonite product is obtained and subjected to reduced-pressure distillation, and a pure product is obtained. According to the method, diethyl methyl-phosphonite is directly prepared from the ternary complex, an intermediate methyl phosphonic dichloride is not needed, and dangerous level of industrial production is reduced; compared with a traditional technology for preparing diethyl methyl-phosphonite from the intermediate methyl phosphonic dichloride, ethyl alcohol and sodium chloride through a reaction, the reaction conditions are milder, waste residue rate is obviously reduced, and yield is as high as 85%.
Methyl asia phosphine acid ester compound synthesis and purification method
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Paragraph 0061; 0062; 0063, (2018/02/04)
The invention relates to a synthesis and purification method of methyl phosphinate compounds. The method concretely comprises the following steps: adding brine to a solution containing a methyldialkyl phosphinate and magnesium chloride mixture in an inert solvent at a low temperature, and separating to obtain methylalkyl phosphinate or methyldialkyl phosphinate. The method solves the post-treatment and purification difficulties of a Grignard reagent method, and has the advantages of industrial production, effective reduction of the generation of methyl phosphonous acid, mild process conditions, and excellent reaction yield and product quality.
Preparation method of dialkyl methylphosphonite
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Paragraph 0047-0054; 0064-0077, (2018/02/04)
The invention relates to a preparation method of dialkyl methylphosphonite. tertiary amine with pKa greater than 10 is adopted as the acid binding agent, methyl phosphonic dichloride and alcohol react in a solvent, and the mole ratio of the methyl phosphonic dichloride, alcohol and tertiary amine is 1:2.0-2.4:2.0-2.4, the produced tertiary amine hydrochloride is neutralized with a caustic soda aqueous solution, and the solvent and tertiary amine obtained by evaporation is recycled and reused. The alkyl of the dialkyl methylphosphonite is straight chain and side chain alkane or alkene of aliphatic C1-C4, the alcohol refers to methanol, ethanol, propanol, isopropanol, allyl alcohol, n-butanol, isobutanol and the like, the tertiary amine refers to tertiary fatty amine, and also refers to fatty group and aromatic mixed tertiary amine, at the same time, the pKa of the tertiary amine is required to be greater than 10, and the tertiary amine can include triethylamine, tripropylamine and tributylamine.
A kind of preparation method for treating keratoconjunctival and wherein the intermediate preparation method
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Paragraph 0117; 0118, (2017/03/08)
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.
Synthetic method of methyl phosphite and glufosinate-ammonium
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Paragraph 0033; 0052, (2016/11/07)
The invention discloses a synthetic method of methyl phosphite and glufosinate-ammonium. The method comprises the steps: with phosphorus pentasulfide as a starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite (III), and next carrying out Grignard reaction to obtain methyl phosphite (IV), wherein R is C1-C4 alkyl. The method comprises the steps: with phosphorus pentasulfide as the starting material, then carrying out vulcanization reaction, chlorination reaction, water washing and distillation purification, then carrying out catalytic hydrogenation to obtain chloride phosphite, next carrying out Grignard reaction to synthesize methyl phosphite (IV), and thus obtaining the final product glufosinate-ammonium through a Strecker route of the prior art. The synthetic yield is increased, methyl phosphorus dichloride and other unstable corrosive intermediates cannot be produced, the discharge of three-waste substances is reduced, and environment-friendly costs and pressure are reduced.
Direct α-chlorination of O,O-dialkyl chalcogenophosphonates with phosphorus oxychloride
Mons, Stéphane,Sabourault, Nicolas,Klein, Emmanuel,Mioskowski, Charles,Lebeau, Luc
, p. 7547 - 7549 (2007/10/03)
α-Chlorination of phosphonates, and O,O-dialkyl thio- and selenophosphonates involving the direct reaction of their lithiated anion with phosphorus oxychloride is described. The reaction gives good results where previously known methods fail. The role of the chalcogen atom, and the influence of the nature of the alkyl chain with respect to the reactivity are discussed.
Synthesis, NMR, relaxometry and circularly polarised luminescence studies of macrocyclic monoamidetris(phosphinate) complexes bearing a remote chiral centre
Aime, Silvio,Botta, Mauro,Dickins, Rachel S.,Maupin, Christine L.,Parker, David,Riehl, James P.,Williams, J. A. Gareth
, p. 881 - 892 (2007/10/03)
Lanthanide complexes of macrocyclic monoamidetris(phosphinate) ligands are partially hydrated in aqueous solution. Introduction of a chiral centre into the amide group leads to the formation of only two non-interconverting complex diastereoisomers (2:1 for α-phenylethyl and 4:1 for α-1-naphthylethyl). Proton, 31P NMR and circularly polarised luminescence studies indicated that the configuration at the chiral carbon centre determines the helicity of the layout of the pendent arms and the macrocyclic ring conformation, with an RRR or SSS configuration preferred at the phosphorus centres.
