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.
Preparation method of dialkyl methylphosphonite
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Paragraph 0038-0045; 0078-0094, (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.