Method for synthesizing diamide podand extraction agent

A technology of diamide pod ether and synthesis method is applied in the field of synthesis of diamide pod ether extractant, and achieves the effects of short time consumption, simple and mature method, and fast reaction speed.

Active Publication Date: 2013-03-27
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] The purpose of the present invention is to solve the problems existing in the existing synthetic method of diamide pod ether extractant, to provide a kind of synthetic method of diamide pod ether extractant with mild synthesis conditions, simple and convenient method, high yield, and suitable for industrialized production

Method used

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  • Method for synthesizing diamide podand extraction agent
  • Method for synthesizing diamide podand extraction agent
  • Method for synthesizing diamide podand extraction agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Add 11.6g (0.1mol) of diglucoside anhydride to 77mL (0.9mol) of 1,4-dioxane, and place it in an ice-water bath at 7°C, while stirring, add 10.2mL (0.1mol) of diethyl The mixture of amine and 8.2mL (0.102mol) of pyridine was reacted for 0.5h after the dropwise addition, the ice-water bath was removed, and then reacted at room temperature for 3h, and then the 1,4-dioxane solvent was removed by rotary evaporation, and the volume ratio It is a 1:1 mixed solution of hydrochloric acid and water, that is, a large number of white crystals are precipitated, then filtered by suction, recrystallized with ether, and dried in vacuum to obtain white flaky crystals of N,N-diethyl-3-oxopentaramic acid 16.9 g, yield 71%.

[0035] 2) Stir and mix 5.67g (0.03mol) N, N-diethyl-3-oxopentaramic acid, 3.3mL (0.03mol) N-methylmorpholine and 280mL tetrahydrofuran and cool to -10°C, drop Add a mixture of 3.9mL (0.03mol) of isobutyl chloroformate and 5mL of tetrahydrofuran, stir for 2 minutes...

Embodiment 2

[0037] 1) Add 11.6g (0.1mol) of diglucoside anhydride to 96mL (15mol) of dichloromethane, and place in an ice-water bath at 3°C, while stirring, add 10.7mL (0.105mol) of diethylamine and 10.4mL (0.13 mol) the mixed solution of pyridine, react 1h after dropwise addition, remove the ice-water bath, react at room temperature for 5h, and then rotary evaporation removes the methylene chloride solvent and then dropwise add the mixed solution of hydrochloric acid and water with a volume ratio of 1:1, That is, a large amount of white crystals were precipitated, which were then suction filtered, recrystallized with ether, and dried in vacuo to obtain 12.8 g of white flaky crystals of N,N-diethyl-3-oxopentaramic acid, with a yield of 54%.

[0038] 2) Stir and mix 1.89g (0.01mol) N, N-diethyl-3-oxopentaramic acid, 2.8mL (0.02mol) triethylamine and 60mL dichloromethane and cool to -15°C, then drop Add 1mL (0.0103mol) of a mixture of ethyl chloroformate and 1mL of dichloromethane, stir the...

Embodiment 3

[0040] 1) Add 11.6g (0.1mol) of diglycolic anhydride to 105mL (13mol) of tetrahydrofuran, and place it in an ice-water bath at 4°C, while stirring, add 10.5mL (0.103mol) of diethylamine and 9.3mL (0.115mol) of diethylamine dropwise. The mixed solution of pyridine was reacted for 0.5h after the dropwise addition, the ice-water bath was removed, and then reacted at room temperature for 3.5h, and then the tetrahydrofuran solvent was removed by rotary evaporation, and the mixed solution of hydrochloric acid and water with a volume ratio of 1:1 was added dropwise thereto, that is, A large number of white crystals were precipitated, and then filtered by suction, recrystallized with ether, and dried in vacuum to obtain 16.2 g of white flaky crystals of N,N-diethyl-3-oxopentaramic acid, with a yield of 68%.

[0041] 2) Stir and mix 2.835g (0.015mol) N,N-diethyl-3-oxopentaramic acid, 2.3mL (0.0165mol) N,N-dimethylethylamine and 70mL dimethylformamide and Cool to -11°C, then add dropwis...

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Abstract

The invention discloses a method for synthesizing diamide podand extraction agent, wherein chloro-carbonic ester and diglycolic anhydride react to generate mixed anhydride under the action of tertiary amine, and then the reaction is performed with amine to generate the diamide podand extraction agent. The method has mild reaction condition, can be performed at a low temperature, and has high reaction speed and short consumed time; the product purification operation is simple and easy; the obtained diamide podand extraction agent can meet the extraction purity requirement, and is beneficial to establishing flow that the diamide podand is used for treating high-level liquid waste in spent fuel reprocessing plant; the used chloro-carbonic ester is easy to prepare and has a low price, therefore, the cost for preparation of a great amount of extraction agent is greatly reduced; and besides, the yield of the extraction agent is high, so that the method is very suitable for industrial production and application.

Description

technical field [0001] The invention belongs to the technical field of preparation of diglycoside amide compounds in organic chemistry, and in particular relates to a synthesis method of a diamide podyl ether extractant used in spent fuel reprocessing. Background technique [0002] Amide pod ether is a new type of neutral complex extractant developed in recent years. Its chemical structure is as follows: [0003] [0004] In the formula, when the substituent R is a methyl group, an ethyl group, or a propyl group, the corresponding amide pod ether is a water-soluble compound, which can be used as a stripping agent for the extracted metal ions in the solvent extraction process for the aqueous reprocessing of spent fuel ( Zhang Ping, Chen Jing, Tian Guoxing, et al. A Method for Separating Radioactive Elements from Organic Reverse Extraction with Water-Soluble Oxaamides. China 03146394.0[P].2004.02.25; Sasaki Y, Sugo Y, Kitatsuji Y, et al.Complexation and back extraction of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/06C07C231/02
Inventor 丁颂东吴宇轩刘宁黄松黄璜苏冬萍王洁茹谈梦玲
Owner SICHUAN UNIV
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