Method for synthesizing methoxy acetone

A technology of methoxyacetone and methoxyl group, applied in the field of synthesis of methoxyacetone, can solve the problems of difficult recovery, difficult oxidation of 1-methoxy-2-propanol, difficult product separation, etc., and achieves easy industrialization The effect of mild production and reaction conditions

Inactive Publication Date: 2016-07-20
DALIAN SYNCO CHEM CO LTD
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Problems solved by technology

At present, the synthesis method of methoxyacetone is mainly obtained by oxidation of 1-methoxy-2-propanol as a raw material, but due to the formation of intramolecular hydrogen bonds and the electron-withdrawing effect of methoxy, 1-methoxy -2-propanol is difficult to oxidize
[0003] In the synthetic methods reported in the literature and patents, there is a liquid phase reaction Na 2 WO 4 -H 2 o 2 , Pt / C and other systems, the conversion rate and selectivity are not very high, the catalyst is expensive, and it is difficult to recycle a series of problems
Simultaneously, because raw material 1-methoxyl-2-propanol and methoxyacetone boiling point are very close, cause product separation more difficult, make product content difficult to reach very high

Method used

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  • Method for synthesizing methoxy acetone

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Experimental program
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Effect test

Embodiment 1

[0014] In the 1000ml four-necked reaction flask (with mechanical stirring, thermometer, dropping funnel and reflux condenser), add 90 grams of 1-methoxyl-2-propanol, then add 360 grams of dichloromethane, then add 0.47 grams of TEMPO , then add 96.6 grams of sodium bicarbonate, lower the temperature to 0-10°C, and gradually add 81.4 grams of oxidant TCIA. During this process, use an ice-salt bath to cool down, so that the temperature is maintained at 0-10°C, and the addition is completed within 3 hours. Afterwards, the reaction was continued for 0.5 hours, and samples were taken for gas chromatography (GC) analysis of raw material content (<0.5%). After the reaction was completed, the reaction solution was filtered, and the filter cake was washed with 100 grams of dichloromethane. After the mother liquor and washing liquid were combined, they were concentrated, the dichloromethane was recovered, and then vacuum distillation was carried out to obtain methoxyacetone: 86.1 grams, ...

Embodiment 2

[0016] In the 1000ml four-necked reaction flask (with mechanical stirring, thermometer, dropping funnel and reflux condenser), add 90 grams of 1-methoxyl-2-propanol, then add 400 grams of dichloromethane, then add 0.47 grams of TEMPO , then add 96.6 grams of sodium bicarbonate, lower the temperature to 10-20°C, and gradually add 81.4 grams of oxidizing agent TCIA. During this process, use an ice-salt bath to cool down, keep the temperature at 10-20°C, and finish adding within 3 hours. The reaction was continued for 0.5 hours, and a sample was taken for GC analysis of the raw material content (<0.5%). After the reaction, the reaction solution was filtered, and the filter cake was washed with 100 grams of dichloromethane. After the mother liquor and washing liquid were combined, they were concentrated, and the dichloromethane was recovered, and then vacuum distillation was carried out to obtain methoxyacetone: 85.5 grams, GC content: 99.7%, yield: 97.2%.

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Abstract

The invention belongs to the technical field of chemistry and chemical engineering, and particularly relates to a method for synthesizing methoxy acetone.The method is a catalytic oxidation method, and 1-methoxy-2-propyl alcohol, chlorohydrocarbon, a nitroxide free radical, sodium bicarbonate and trichloroisocyanuric acid are used as a raw material, solvent, a catalyst, an acid-binding agent and an oxidizing agent respectively to conduct a catalytic oxidation reaction.The reaction product is filtered after the reaction is completed, filter liquor is concentrated to recover solvent, and methoxy acetone is obtained through distillation.The 100% conversion rate of 1-methoxy-2-propyl alcohol in the reaction process can be nearly realized, the purity of methoxy acetone can reach 99.5% or more, the reaction condition is mild, and the synthetic method has industrial production prospects.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a method for synthesizing methoxyacetone. Background technique [0002] Methoxyacetone is an important fine chemical product, which is mainly used as a raw material for the pesticide metolachlor (Dour) and some pharmaceutical synthesis. As a low-toxicity herbicide, metolachlor has been widely used in northern China of dry fields. At present, the synthesis method of methoxyacetone is mainly obtained by oxidation of 1-methoxy-2-propanol as a raw material, but due to the formation of intramolecular hydrogen bonds and the electron-withdrawing effect of methoxy, 1-methoxy -2-propanol is difficult to oxidize. [0003] In the synthetic methods reported in the literature and patents, there is a liquid phase reaction Na 2 WO 4 -H 2 o 2 , Pt / C and other systems, the conversion rate and selectivity are not very high, the catalyst is expensive, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/30C07C49/175
CPCC07C45/30
Inventor 程宪冷学超刘晨旭王延波
Owner DALIAN SYNCO CHEM CO LTD
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