20278-51-7Relevant articles and documents
Preparation method of monoalkyl phosphinic acid dialkyl ester, dialkyl phosphonate and metal salt thereof
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Paragraph 0049-0050, (2021/02/06)
The invention relates to the technical field of phosphonate synthesis, and discloses a preparation method of monoalkyl phosphinic acid dialkyl ester, which comprises the following steps: reacting monoalkyl phosphonic acid dialkyl ester under the action of a silicon-hydrogen-containing reducing agent to obtain a monoalkyl phosphinic acid dialkyl ester, wherein the reaction formula is shown in the specification, each R1 is independently an alkyl group with 1-10 carbon atoms, and the silicon-hydrogen-containing reducing agent is chlorine-containing and/or hydrogen-containing silane. The inventionalso discloses a method for preparing dialkyl phosphonate by isomerizing the monoalkyl phosphinic acid dialkyl ester, and further discloses a preparation method of dialkyl phosphinic acid and metal salt thereof. The method is mild in process condition and easy to implement in industrialization, aftertreatment is simple and feasible, the product purity reaches up to 98-99%, dialkyl phosphinic acidobtained through hydrolysis of dialkyl phosphonic acid alkyl ester can also be applied to extraction of metal ions or rare earth, and extra purification is not needed.
Method using one-pot method to prepare 4-(methyl hydroxyl phosphoryl)-2-carbonyl butyric acid
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Paragraph 0013; 0023-0032, (2017/08/25)
The invention discloses a method using a one-pot method to prepare 4-(methyl hydroxyl phosphoryl)-2-carbonyl butyric acid. The method is characterized in that methyl phosphorus dichloride is allowed to react with methanol to prepare methyl dimethoxy phosphorus as shown in formula (I), the methyl dimethoxy phosphorus is allowed to directly react with methyl acrylate to prepare a compound as shown in formula (II) without separation and purification, the compound as shown in formula (II) is allowed to have condensation reaction with diethyl oxalate to prepare a compound as shown in formula (III), and the compound as shown in formula (III) is allowed to react with hydrochloric acid to prepare the 4-(methyl hydroxyl phosphoryl)-2-carbonyl butyric acid. The method using the one-pot method to prepare the 4-(methyl hydroxyl phosphoryl)-2-carbonyl butyric acid has the advantages that the steps of the method are orderly connected, the method is short in synthesizing route, high in reaction yield, simple to operate and especially suitable for industrial production, and enterprise market competitiveness is enhanced.
A kind of preparation method for treating keratoconjunctival and wherein the intermediate preparation method
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Paragraph 0119; 0120, (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.