METHOD FOR PREPARING 4-(HYDROXYMETHYLPHOSPHINYL)-2-OXOBUTANOIC ACID
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United States of America
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Mar 13, 2025
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Mar 6, 2023
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Mar 6, 2023
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Abstract
A method for preparing 4-(hydroxymethylphosphinyl)-2-oxobutanoic acid, comprising the following steps: a) mixing 3-chloropropionyl chloride, a first solvent, trimethylsilyl cyanide and cyanide salt, performing a substitution reaction to obtain a material solution containing 4-chloro-2-oxobutyronitrile, then performing distillation under reduced pressure, and performing separation to obtain 4-chloro-2-oxobutyronitrile intermediate; b) subjecting the 4-chloro-2-oxobutyronitrile intermediate obtained in step a) and methyl phosphonite diester to Arbuzov reaction in a second solvent in the presence of cuprous iodide to obtain a material solution of (3-cyano-3-oxopropyl) methyl phosphinate, and performing purification to obtain crude (3-cyano-3-oxopropyl) methyl phosphinate; c) mixing the obtained crude (3-cyano-3-oxopropyl)methyl phosphinate with hydrochloric acid, performing hydrolysis reaction, and then performing purification treatment to obtain 4-(hydroxymethylphosphinyl)-2-oxobutanoic acid. This preparation method can prepare 4-(hydroxymethylphosphinyl)-2-oxobutanoic acid with high yield, and the reaction conditions are mild, the operation is simple, the production cost is low, and it is easy to realize industrialization.
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