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Method for synthesizing diamide compound (R1R2NCO) 2CH2OCH2

A 2CH2OCH2, synthetic method technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of carboxylic acid amides, etc., can solve the problems of large amount of instrument usage, high cost, large amount of waste gas and waste liquid, etc. The effect of low pollution and mild reaction conditions

Inactive Publication Date: 2011-04-20
UNIV OF JINAN
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Problems solved by technology

[0006] The problem that this method exists is: when making acid chloride by diglycidic acid, all reagents must be processed through purification to remove the remaining water and alcohol and other substances that can react with thionyl chloride, and the instruments used must be dried. Use drying tubes to isolate external water vapor from entering the reaction system
Both diglycolyl chloride and 3-oxoglutaramide need to be distilled under reduced pressure to obtain pure products, resulting in a large amount of waste gas and waste liquid, which requires a large amount of equipment and high cost

Method used

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  • Method for synthesizing diamide compound (R1R2NCO) 2CH2OCH2
  • Method for synthesizing diamide compound (R1R2NCO) 2CH2OCH2

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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1N, N, N', the preparation of N'-tetrabutyl-3-oxoglutaramide (TBOPDA)

[0019] 1 Preparation of Diglycolic Acid

[0020]

[0021] Add 1000g of concentrated nitric acid (about 714mL) into a 1000mL three-flask equipped with a constant pressure funnel, a thermometer and a reflux device, heat under magnetic stirring until the temperature in the flask reaches 65°C, stop heating, and drop a few drops of absolute ethanol as a trigger At this time, reddish-brown gas was released in the flask, and 1mol (106mL) diethylene glycol was added under stirring, and the rate of addition was controlled to keep the reaction temperature between 65-70°C. The reaction was violent, and a large amount of reddish-brown gas was released. Absorb with 5% sodium hydroxide solution. After the dropwise addition was completed, the temperature was raised to 80°C until the nitrogen dioxide in the bottle was no longer generated, and 200 mL of distilled water was added to stop the reaction. ...

Embodiment 2

[0033] Embodiment 2: N, N'-dimethyl-N, the preparation of N'-diphenyl-3-oxyglutaramide (DMDPhOPDA)

[0034] The preparation of diglycolic acid and dimethyl diglycidate is the same as in Example 1.

[0035] N, N'-dimethyl-N, the preparation reaction formula of N'-diphenyl-3-oxyglutaramide (DMDPhOPDA) is:

[0036]

[0037] Add 32.43g dimethyl diglycidate (0.2mol, 162.14g mol-1) and 53.5g N-methylaniline (0.5mol, 107.15g mol-1) into a three-necked flask, with a magnetic stirrer and oil bath, top-mounted thermometer and reflux condenser. Slowly heat to a temperature of about 50°C, all the solids in the flask melt, start stirring, and control the temperature at 160°C for reaction. The reaction was stopped after the completion of the reaction detected by thin-layer chromatography, and it took about 4-6 hours.

[0038] After the reaction is completed, filter and distill off methanol and unreacted N-methylaniline under reduced pressure. After diluting the remaining substance wit...

Embodiment 3

[0039] Embodiment 3: N, N'-dimethyl-N, the preparation of N'-diphenyl-3-oxyglutaramide (DMDPhOPDA), used N-methylaniline gets 0.4mol, other is with embodiment 2.

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Abstract

The invention discloses a novel method for synthesizing a diamide compound (R1R2NCO) 2CH2OCH2, which comprises the following steps of: with a hydrogen chloride gas as a catalytic agent, catalyzing diglycolic acid and methanol to prepare diglycolic acid dimethyl ester; and reacting the diglycolic acid dimethyl ester with amine to produce the corresponding 3-oxa-pentanediamide. Reaction conditions are mild, and operation steps are simple because of omitting the preparation of acyl chloride; the prepared ester can be stored for long, which is convenient for increasing production efficiency; environment pollution is lower without exhausting a large quantity of sulfur dioxide or hydrogen chloride gas.

Description

technical field [0001] The invention belongs to the technical field of extraction of rare earth elements, and in particular relates to a novel extractant (R 1 R 2 NCO) 2 CH 2 OCH 2 synthetic method. Background technique [0002] my country is the main rare earth resource country and the only country that can provide all 17 kinds of rare earth metals. Its proven reserves rank first in the world, and its output and supply reach 80% to 90% of the world's total. At present, the state has increased the control and management of rare earth mining. At the same time, the mining, separation and application of rare earth have also been greatly developed under the attention of researchers. As rare earth elements play an important role in various fields of industry, the requirements for high-purity single rare earth elements are getting higher and higher. However, rare earths are very difficult to separate due to their similar structures and most of them exist as paragenetic ores....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C235/16C07C235/06
Inventor 崔玉杨玉兰孙国新夏光明聂永
Owner UNIV OF JINAN
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