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Green synthesis method for ketazine

A green synthesis and ketazine technology, which is applied in the preparation of hydrazones and organic chemistry, can solve the problems of increased production costs, achieve good thermal stability, and be easy to recycle and recycle.

Inactive Publication Date: 2008-08-06
山东兴安智慧科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of ionic liquids increases production costs, and new problems need to be solved for the preparation of ketazine

Method used

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  • Green synthesis method for ketazine
  • Green synthesis method for ketazine
  • Green synthesis method for ketazine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Acetamide (5.9g, 0.1mol), sodium hexametaphosphate (0.3g, 0.0005mol), acetonitrile (10.5mL, 0.20mol), polyethylene glycol were added successively into a 100mL three-necked round-bottomed flask equipped with a thermometer and a condenser. Alcohol 6000 (1g, 0.0002mol), methyl ethyl ketone (36mL, 0.40mol), add dropwise 25% (w / w) ammonia water (18.0mL, 0.20mol), 30% (w / w) hydrogen peroxide (10.22mL , 0.10mol), stirred at 40°C for 8 hours, separated with a separatory funnel, separated the organic layer, and distilled to obtain 10.03 grams of methyl ethyl ketazine (I-1), with a yield (calculated as hydrogen peroxide) of 71.7%.

[0047]

Embodiment 2

[0049] Acetamide (5.9g, 0.1mol), sodium hexametaphosphate (0.3g, 0.0005mol), acetonitrile (10.5mL, 0.20mol), polyethylene glycol were added successively into a 100mL three-necked round-bottomed flask equipped with a thermometer and a condenser. Alcohol 6000 (1g, 0.0002mol), acetone (29.5mL, 0.40mol), add dropwise 25% (w / w) ammonia water (18.0mL, 0.20mol), 30% (w / w) hydrogen peroxide (10.22mL , 0.10mol), stirred at 40°C for 8 hours, added solid sodium hydroxide in an ice-water bath until saturated, kept the temperature not exceeding 30°C during the period, left the solution to separate layers, separated with a separatory funnel, separated the organic layer, and distilled 8.46 g of acetonazine (I-2) was obtained, and the yield (calculated as hydrogen peroxide) was 75.6%.

[0050]

Embodiment 3

[0052] Acetamide (5.9g, 0.1mol), sodium hexametaphosphate (0.3g, 0.0005mol), acetonitrile (10.5mL, 0.20mol), polyethylene glycol were added successively into a 100mL three-necked round-bottomed flask equipped with a thermometer and a condenser. Alcohol 400 (1g, 0.0025mol), methyl ethyl ketone (36mL, 0.40mol), add dropwise 25% (w / w) ammonia water (18.0mL, 0.20mol), 30% (w / w) hydrogen peroxide (10.22mL , 0.10mol), stirred at 70°C for 5 hours, separated with a separatory funnel, separated the organic layer, and distilled to obtain 11.28 grams of methyl ethyl ketazine, with a yield (calculated as hydrogen peroxide) of 80.6%.

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Abstract

The invention provides an environment-friend synthesis method of azine, which comprises synthesizing ammonia, hydrogen dioxide and ketone in the reaction system of catalyst and carbowax at 10-100DEG C, separating water phase and organic phase, distilling the organic phase, and purifying via decompresson and recrystallization to obtain azine product. The environment-friend synthesis method of azine utizlies carbowax which has high thermal stability, is not volatile, inflammable and toxic, is bio-degradable, cheap and easy to get, easy to recover and circulate, with high product yield. The acetonitrile of organic phase in reaction, unreacted ketone, the catalyst in water phase and unreacted ammonia can be recovered without effect on reaction yield.

Description

(1) Technical field [0001] The invention relates to a green synthesis method of ketazine. (2) Background technology [0002] Ketone azine is an important intermediate product in the preparation of hydrazine hydrate by hydrolysis. At present, the production of ketazine by hydrogen peroxide method is considered to be the most economical and practical advanced technology, and it is also a green 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 ketazine to prepare hydrazine hydrate is of great significance. [0003] As we all know, hydrazine hydrate is an important chemical raw material and has a wide range of uses. Since the hydrazine hydrate molecule contains two nucleophilic nitrogens and four replaceable hydrogens, the fine chemical products using hydrazine hydrate as raw materials involve almost all fields. . The pharmaceutical industry is often used to produ...

Claims

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Application Information

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IPC IPC(8): C07C251/88C07C249/16
Inventor 裴文段江丽王菊华
Owner 山东兴安智慧科技有限公司
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