Synthesis process of methyl ethyl ketone azine

A technology for the synthesis of methyl ethyl ketone and its synthesis method, which is applied in the field of synthesis of methyl ethyl ketazine, can solve the problems of reduced yield and difficult product separation, and achieve increased yield, high product yield, and good dissolution sexual effect

Inactive Publication Date: 2005-12-14
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, when this method is synthesizing ketazine, the impurity that side reaction generates is recovered together with unreacted ketone and reuses, and the yield of synthesizing ketazine is gradually reduced due to the accumulation of impurities, resulting in difficulty in product separation

Method used

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  • Synthesis process of methyl ethyl ketone azine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 Synthesis of methyl ethyl ketazine in 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid

[0046] Add cyanoacetamide (6g, 71.4mmol), 1-butyl-3-methylimidazolium tetrafluoroborate (20ml), sodium hexametaphosphate ( 0.6g, 1.0mmol), acetonitrile (20ml, 586mmol), 28% (mass content) of ammonia (50ml, 588mmol), butanone (54ml, 588mmol), dropwise 30% (mass content) of hydrogen peroxide (20ml , 196mol), stirred at 40°C for 8 hours, distilled the reaction solution, steamed off ammonia, butanone, acetonitrile, 2-butanol, water, and extracted the remaining liquid with dichloromethane to recover the ionic liquid to obtain 16.05g of the product, the yield 58.6% (calculated as hydrogen peroxide).

Embodiment 2

[0047] Example 2 Synthesis of methyl ethyl ketazine in 1-benzyl-3-methylimidazolium tetrafluoroborate ionic liquid

[0048] Add cyanoacetamide (3g, 35.7mmol), 1-benzyl-3-methylimidazolium tetrafluoroborate (10ml), sodium hexametaphosphate ( 0.3g, 0.5mmol), acetonitrile (10ml, 293mmol), 28% (mass content) of ammonia (25ml, 294mmol), methyl ethyl ketone (27ml, 294mmol), dropwise 30% (mass content) of hydrogen peroxide (10ml , 98mmol), stirred at 50°C for 8 hours, distilled the reaction solution, steamed off ammonia, butanone, acetonitrile, 2-butanol, water, and extracted the remaining liquid with dichloromethane to recover the ionic liquid to obtain 7.74g of the product, the yield 56.5% (calculated as hydrogen peroxide).

Embodiment 3

[0049] Example 3 Synthesis of methyl ethyl ketazine in 1-butyl-3-methylimidazole acetate ionic liquid

[0050] Add cyanoacetamide (3g, 35.7mmol), 1-butyl-3-methylimidazole acetate (10ml), sodium hexametaphosphate (0.3g , 0.5mmol), acetonitrile (10ml, 293mmol), 28% (mass content) ammonia (25ml, 294mmol), butanone (27ml, 294mmol), hydrogen peroxide (10ml, 98mmol) was added dropwise, and stirred at 45°C for 6 Hours, the reaction solution was distilled to remove ammonia, butanone, acetonitrile, 2-butanol, and water, and the remaining liquid was extracted with toluene to recover the ionic liquid to obtain 12.03 g of the product with a yield of 87.8% (based on hydrogen peroxide).

[0051] The ionic liquid in the reaction system can continue to be recycled.

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Abstract

The synthesis process of methyl ethyl ketone azine includes the synthesis of ammonia, hydrogen peroxide and methyl ethyl ketone in work solution containing catalyst and ionic liquid at 20-100 deg.c, and post-treatment to obtain product. The synthesis process inside ionic liquid of the present invention has high safety, high dissolubility on organic matter and inorganic matter, homogeneous reaction condition, easy operation and treatment, and high product yield. The ammonia water, methyl ethyl ketone and methyl cyanide distilled out of the reacted liquid may be reused without influence on the yield.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing methyl ethyl ketazine. (2) Background technology [0002] Methyl ketone azine is an important intermediate product in the preparation of hydrazine hydrate, and high-quality hydrazine hydrate can be obtained in high yield through hydrolysis. At present, the use of hydrogen peroxide to produce methyl ethyl ketazine is considered to be the most economical and practical advanced technology, and it is also a green chemical synthesis technology. The technology is simple to operate, short in reaction time, easy to obtain raw materials, low in cost, and high in product yield. The use of methyl ethyl ketazine to prepare hydrazine hydrate is of great significance. [0003] As we all know, hydrazine hydrate is a widely used chemical with multiple uses, mainly used in the synthesis of pesticides and medicines, water treatment agents and polymer foaming agents, and plays an important role in high-tech fields s...

Claims

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Application Information

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IPC IPC(8): C07C251/08
Inventor 裴文孙孟展赵尚原马波张才
Owner ZHEJIANG UNIV OF TECH
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