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Synthesis of water soluble oxamonoamide

A technology for the synthesis of oxamonoamides, which is applied to the preparation of carboxylic acid amides, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as low yield, limited industrial application, and difficult separation, and achieve high yield , The effect of easy product and simple process

Inactive Publication Date: 2005-05-11
TSINGHUA UNIV
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Problems solved by technology

Generally, there are few reports on the synthetic method of oxamonoamide compounds. The existing synthetic method is to directly react acid anhydride and dialkylamine under reflux conditions, and generally obtain a mixture of oxamonoamide, pod ether and diglycolic acid. Low yield and difficult separation limit its industrial application

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  • Synthesis of water soluble oxamonoamide

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Embodiment Construction

[0008] The invention proposes a synthesis method of water-soluble oxamonoamide. The method uses diethylene glycol as a raw material, undergoes oxidation and condensation to obtain diglycolic anhydride, and then reacts with dialkylamine to obtain amide. Its reaction formula is as follows:

[0009]

[0010] The synthesis method is divided into three steps:

[0011] (1) diethylene glycol prepares diglycolic acid: diethylene glycol is oxidized to diglycolic acid through concentrated nitric acid (concentration is 10mol / L), (the volume ratio of diethylene glycol and concentrated nitric acid is 1: 7~10);

[0012] (2) Diglycolic acid generates diglycolic anhydride: Diglycolic acid and acetic anhydride (molar ratio is 1:5~7) are reacted and crystallized with toluene to obtain white diglycolic anhydride crystals; Dosage plus toluene;

[0013] (3) Synthesis of oxamonoamide: Diglycolic anhydride is reacted with dimethylamine, diethylamine or dipropylamine (molar ratio is 1:1) respect...

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Abstract

Synthesis of water soluble half amide oxide is carried out by taking 1,4-dioxane as solvent at low-temperature, diethylene acid anhydride reacting with dimethylamine, diethylamine, and dipropylamine under pyridine, the products concentrating, chlorhydric acid acidifying, crystallizing precipitating, and annealing purifying in water or alcohol and diethyl ether mixed solvent. Its advantages include good water solubility, high output, and simple process.

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 synthesis method of a water-soluble oxamonoamide used in nuclear fuel post-treatment, high-level radioactive waste liquid treatment and nuclide decontamination. Background technique [0002] For the ester-soluble extractant macrocyclic crown ether and pod ether, there have been many studies on their synthesis methods, and they have been applied to the extraction of certain metal ions and radionuclides. In recent years, studies have found that oxamonoamide compounds have excellent coordination ability to metal ions like crown ethers and pod ethers. The difference is that they have good water solubility. Using these properties, they can be used as stripping agents. Generally, there are few reports on the synthetic method of oxamonoamide compounds. The existing synthetic method is to directly react acid anhydride and dialkyla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/10C07C235/04
Inventor 王海荣张平王建晨陈靖
Owner TSINGHUA UNIV
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