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Preparation method of alpha-hydroxyl ketone compounds

A compound and hydroxyketone technology, applied in the preparation of organic compounds, carbon-based compounds, chemical instruments and methods, etc., can solve problems such as difficult to realize industrial production, and achieve stable product quality, short reaction time and simple process Effect

Active Publication Date: 2011-04-06
HUNAN HONGBANG NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its synthesis method is also: first prepare sodium sand, at a temperature of 10-45 ° C, the sodium sand in the solvent and fatty acid ester undergo an azoin condensation reaction, and the preparation of sodium sand requires heating, and then rapid stirring and quenching, every At the same time, only a small amount of sodium sand can be prepared in the laboratory. Similarly, there will be a difficult problem that rapid stirring and quenching are not easy to achieve in actual production, so it is also difficult to realize industrial production

Method used

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  • Preparation method of alpha-hydroxyl ketone compounds
  • Preparation method of alpha-hydroxyl ketone compounds
  • Preparation method of alpha-hydroxyl ketone compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0030]Example 1: In a four-necked 1-liter reactor equipped with a stirrer, reflux condenser, dropping funnel, and temperature sensor, add 300ml of toluene, then add 15.8g of sodium metal to remove surface oxides, heat up and heat until the sodium melts , start stirring until the sodium turns into fine particles, and the rotating speed is 750 rpm; when the temperature of the mixture in the reactor reaches 107°C, maintain the temperature, and add dropwise a mixture of 200ml of toluene and 50ml of methyl isooctanoate under stirring. After the dropwise addition, the reaction mixture changed from blue-yellow to brown-yellow, and the reaction mixture became thicker. Control the dropping speed, and drop feed liquid within 2 hours. After stirring and keeping warm for 0.5 hour, the reacted mixture was cooled to room temperature, and unreacted metal sodium pieces were taken out. Slow first and then fast, carefully control the dropwise addition of 150ml of sulfuric acid with a concentra...

experiment example 2

[0031] Experimental Example 2: In a four-necked 1-liter reactor equipped with a stirrer, reflux condenser, dropping funnel, and temperature sensor, add 300ml of xylene, then add 16.8g of sodium metal that removes surface oxides, and heat up to sodium Melt, start stirring until the sodium turns into fine particles, the rotation speed is 750 rpm; when the temperature of the mixture in the reactor reaches 105°C, maintain the temperature, and add dropwise the mixture consisting of 200ml xylene and 50ml ethyl octanoate while stirring. After the dropwise addition, the reaction mixture changed from blue-yellow to brown-yellow, and the reaction mixture became thicker. Control the dropping speed, and drop feed liquid within 2 hours. After stirring and keeping warm for 1 hour, the reacted mixture was cooled to room temperature, and unreacted metal sodium pieces were taken out. Slow first and then fast, carefully control the dropwise addition of 160ml hydrochloric acid for transformatio...

experiment example 3

[0032] Experimental Example 3: In a four-necked 1-liter reactor equipped with a stirrer, reflux condenser, dropping funnel, and temperature sensor, add 300ml of toluene, then add 14.8g of metallic sodium to remove surface oxides, heat up and heat until the sodium melts , start stirring until the sodium turns into fine particles, and the rotation speed is 750 rpm; when the temperature of the mixture in the reactor reaches 110°C, maintain the temperature, and add dropwise a mixture of 200ml toluene and 50ml methyl stearate under stirring. After the dropwise addition, the reaction mixture changed from blue-yellow to brown-yellow, and the reaction mixture became thicker. Control the dropping speed, and drop feed liquid within 2 hours. After stirring and keeping warm for half an hour, the reacted mixture was cooled to room temperature, and unreacted metal sodium pieces were taken out. Slow first and then fast, carefully control the dropwise addition of 160ml of nitric acid for tra...

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PUM

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Abstract

The invention discloses a preparation method of alpha-hydroxyl ketone compounds, which comprises the following steps: (1) adding sodium metal into an inert organic solvent, heating to 97-140 DEG C to melt sodium metal, and stirring the sodium metal to obtain fine particles; (2) keeping the temperature, and dropwise adding the mixture of inert organic solvent and alkyl fatty acid ester while stirring; and (3) after dropwise addition, keeping the temperature to react, cooling the mixture after reaction to room temperature, dropwise adding an acid to transform, standing until the mixture delaminates, washing the oil phase, drying, and distilling under reduced pressure to obtain the alpha-hydroxyl ketone compounds. The invention does not need to independently prepare sodium sand, and has the advantages of short reaction time, high product yield, simple technique, high safety and reliability, high production efficiency and stable product quality. The invention does not need to quickly stiror quench, and also does not need to independently prepare sodium sand, thereby solving the problem of large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of an intermediate in the field of chemical industry and metallurgical industry, and further relates to a preparation method of α-hydroxyketone compounds. Background technique [0002] α-Hydroxyketone compounds are intermediates for the synthesis of α-Hydroxyketoxime. The agent is applied in the field of solvent extraction to extract Cu 2+ 、Ni 2+ 、Co 2+ and other metal ions have excellent synergistic extraction properties. Such as 5,8-diethyl-7-hydroxy-dodecane-6-oxime, English name: 5,8-Diethyl-7-Hydroxy-6-Dodecanone-0xime, trade name Lix63. [0003] α-Hydroxyketone compounds are intermediates for the synthesis of α-Hydroxyketone oxime, and its synthesis method is the azoin condensation method. For example, the classic synthesis method of 5,8-diethyl-7-hydroxyl-dodecan-6-one has literature abroad [l.Olszan-owski, Andrzej.Production of5,8-Diethyl-7-Hydroxy-6 -DodecanoneOxime.Przem.Chem.1981, 60 (11-12...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/54C07C49/17
Inventor 曹佐英肖连生李青刚张贵清王金明曾理肖超张晓峰
Owner HUNAN HONGBANG NEW MATERIAL
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