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.
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.