Synthesis method for water-soluble bisamide oxide

The technology of an oxamide and a synthesis method is applied in the field of synthesis and purification of water-soluble oxabiamide, and can solve the problems of difficult separation and purification, purification, and the extraction method cannot be used, and achieves high yield, convenient product purification, The effect of excellent coordination properties

Inactive Publication Date: 2005-10-26
TSINGHUA UNIV
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Problems solved by technology

At present, there are few reports on the synthesis and application of short-chain water-soluble oxaamide-type crown ethers. Due to their water solubility, subsequent treatment cannot be purified by extraction, and the synthesis is often monoamide and bisamide. Simultaneously generated, its separation and purification is the difficulty in the synthesis of such substances

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  • Synthesis method for water-soluble bisamide oxide

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[0021] For the preparation of ethylbisamide, diglycolyl chloride and 1,4-dioxane are mixed, and the mixture of diethylamine and pyridine is directly added dropwise under temperature control in an ice-salt bath. After reacting for 3-5 hours, the filtrate was concentrated and dissolved in dichloromethane, fed with ammonia gas for supersaturation, suction filtered again, and the filtrate was concentrated to obtain the product ethyl bisamide.

[0022] 1). Preparation of diglyceric acid: first add deionized water and nitric acid in deionized water with a volume ratio of 1:2~3 of nitric acid with a concentration of 10mol / L to obtain a nitric acid solution, and then add the nitric acid solution dropwise into the nitric acid solution Diethylene glycol or ethanol with a volume of 0.15-2 is oxidized to obtain crystallized diglycolic acid, and excess nitric acid is evaporated. When brownish-yellow smoke is produced, add an appropriate amount of deionized water. Repeat this process until ...

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Abstract

The method for synthesizing water-soluble oxabisamide uses diethylene glycol as raw material, makes said raw material undergo the processes of oxidation and chloridization to obtain diethylene aryl chloride, then makes it react with dialkylamine to obtain bisamide, in the presence of pyridine uses 1,4-dioxane as solvent, and makes diethylene acyl chloride respectively react with dimethylamine or diethylamine or dipropylamine under the condition of low temperature, and makes the obtained product undergo the processes of filtration and aminolysis to make the product separated and purify so as to obtain oxabisamide compound.

Description

technical field [0001] The invention belongs to the technical field of preparation of amide compounds in organic chemistry, and in particular relates to a method for synthesizing and purifying a water-soluble oxabisamide used in nuclear fuel post-treatment and high-level radioactive waste liquid treatment. Background technique [0002] Oxabisamide compounds belong to open-chain crown ethers, which are similar to macrocyclic crown ethers and have good coordination properties with metal ions. Utilizing this performance, it is usually used as the active material of the ion-selective electrode or as the extraction agent of metal ions, and there are many applications in these aspects. There have been many reports on the synthesis of amide crown ethers for this purpose. Almost all of these amide crown ethers are ester-soluble crown ethers, which are long-chain or aromatic amides. Anhydrous benzene is usually used as a solvent for the acylation reaction. Since it is insoluble in w...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/06
Inventor 王海荣张平王建晨陈靖
Owner TSINGHUA UNIV
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