Solvent-free solid-phase catalyzed method for synthesizing hydroxyphosphonate

Abstract

The invention discloses a method for solvent-free solid phase catalytic synthesis of hydroxyl phosphonic acid ester, and belongs to the field of organic chemistry. According to the structure of the hydroxyl phosphonic acid ester, R1 is hydrogen or C1-5 alkyl group or phenyl group, R2 is hydrogen or C1-alkyl group or phenyl group, R1 and R2 form a 3-5-membered heterocyclic ring, and R3 is methyl or ethyl or propyl group or isopropyl or butyl or isobutyl. The synthetic method comprises the steps that ketone or aldehyde compounds, phosphite ester and solid catalysts are heated to enable compounds with raw materials including carbonyl to be melted, and stirring and reactions are carried out; the compounds are cooled to be indoor temperature, solvents are added, and the hydroxyl phosphonic acid ester is obtained through filtering and recrystallization. The method has the advantages that the technological process is simple, the catalysts and the solvents can be recycled and reused, production cost is low and the quality of the hydroxyl phosphonic acid ester is high, and is suitable for the industrialized synthesis of the hydroxyl phosphonic acid ester.

Description

technical field [0001] The invention relates to a method for synthesizing hydroxyphosphonate, in particular to a solvent-free solid-phase catalytic synthesis of hydroxyphosphine [0002] An ester method belongs to the field of organic chemistry. Background technique [0003] Hydroxyphosphonate compounds have important biological activities and are widely used in enzyme inhibitors, anti-virus, anti-parasite, anti-AIDS and other drugs. Hydroxyphosphonate compounds are also important raw materials for the synthesis of hydroxyphosphonate derivatives . The traditional method for synthesizing quaternary carbohydroxyphosphonate compounds is to obtain them under the catalysis of various bases. However, strong bases make it difficult for base-sensitive ketones to obtain target compounds, and the products are easily rearranged to form by-products. Recently, triethylamine, tetraisopropyl titanate, potassium hydrogen phosphate, metal amino complexes, and 2,6-pyridinedicarboxylic acid...

AI Technical Summary

Problems solved by technology

However, the reaction conditions are harsh, the catalyst is highly toxic or the preparation process and operation process are complicated

[0004] Based on various documents and related patents, the synthesis of hydroxyphosphonate still has a small yield, and the following shortcomings are common: the strong base catalyst rearranges hydroxyphosphonate into phosphate, the catalyst is highly toxic, deliquescent, difficult to synthesize, and the synthesis process is difficult. A large amount of solvent is required, a lot of waste water is generated, and it is difficult to scale up the reaction

For this reason, it is necessary to improve its synthesis process, explore the reaction under solvent-free conditions, and catalyze it with solid-phase catalysts. Not only does it not produce a lot of waste water, but the catalyst and solvent can be recycled and reused. The catalyst is stable and cheap and easy to get. No relevant reports have been seen.

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