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Novel methyl heptanone synthesis method

A technique for the synthesis of methyl heptanone, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of low selectivity, improve reaction yield, avoid condensation reaction, The effect of reducing production costs

Active Publication Date: 2015-11-11
JILIN BEISHA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] European patent EP0816321 and Chinese patent CN97120582 disclose a kind of acetone as a substrate, and then pump in isovaleraldehyde and 2% sodium hydroxide aqueous solution through a high-pressure metering pump, synthesize methyl heptenone by condensation reaction, and then hydrogenate Reaction synthesis of methyl heptanone, the invention patent reports the use of 2% sodium hydroxide as a catalyst for the condensation reaction. It will also undergo condensation reaction itself to generate corresponding by-products, resulting in relatively low selectivity of the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] Add 146g of triethylamine and 3g of 5% palladium carbon to a 5L autoclave, seal the reaction system, pass nitrogen to replace the air in the reaction system three times, control the temperature at about 95°C, and pass in hydrogen to control the hydrogen pressure at 8kg / cm 2 Left and right, start stirring and control 500rpm / min, feed at a constant speed through a high-pressure metering pump, continuously pump isovaleraldehyde (1720g, 20mol, 1.0eqV) into acetone (1195g, 20.6mol, 1.0eqV), control the feeding speed, The feeding is completed in about 2 hours. After the feeding is completed, react at this temperature and pressure for about 1 hour. The end point of the reaction is detected by gas chromatography, and the residual amount of isovaleraldehyde is controlled below 0.1%. The content is more than 96%, the content of methyl isobutyl ketone (MIBK) is about 0.5%, and the content of triethylamine is about 3%. Apply mechanically, generate a small amount of water in the rea...

example 2

[0036] Add 146g of triethylamine and 3g of 5% palladium carbon to a 5L autoclave, seal the reaction system, pass nitrogen to replace the air in the reaction system three times, control the temperature at about 95°C, and pass in hydrogen to control the hydrogen pressure at 8kg / cm 2 Around, start stirring and control 500rpm / min, feed at a uniform speed through a high-pressure metering pump, continuously pump isovaleraldehyde (1720g, 20mol, 1.0eqV) into acetone (1218g, 21mol, 1.0eqV), control the feeding speed, about After 2 hours of feeding, after the feeding is over, react at this temperature and pressure for about 1 hour, and detect the reaction end point by gas chromatography, control the residual amount of isovaleraldehyde to be ≤0.1%, and control the content of methyl heptanone in the middle The content of methyl isobutyl ketone (MIBK) is about 0.5%, and the content of triethylamine is about 3%. After the reaction, the reaction system is cooled to room temperature, filtered,...

example 3

[0038] Add 146g of triethylamine and 3g of 5% palladium carbon to a 5L autoclave, seal the reaction system, pass nitrogen to replace the air in the reaction system three times, control the temperature at about 95°C, and pass in hydrogen to control the hydrogen pressure at 8kg / cm 2Left and right, start stirring and control 500rpm / min, feed at a uniform speed through a high-pressure metering pump, continuously pump isovaleraldehyde (1720g, 20mol, 1.0eqV) into acetone (1195g, 21.4mol, 1.0eqV), and control the feeding speed, The feeding is completed in about 2 hours. After the feeding is completed, react at this temperature and pressure for about 1 hour. The end point of the reaction is detected by gas chromatography, and the residual amount of isovaleraldehyde is controlled below 0.1%. The content is more than 96%, the content of methyl isobutyl ketone (MIBK) is about 0.5%, and the content of triethylamine is about 3%. Applied mechanically, a small amount of water is generated in...

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Abstract

The present invention relates to an organic matter synthesis method, particularly to a novel methyl heptanone synthesis method, wherein isovaleraldehyde and acetone are adopted as raw materials and are subjected to an aldol condensation reaction and a hydrogenation reaction through a one-pot method under catalysis of catalysts such as triethylamine and palladium carbon to synthesize the methyl heptanone, a small amount of the by-product methyl isobutyl ketone is subjected to distillation recovery, the recovered product is supplied for other positions, and the catalyst used in the reaction process can be repeatedly applied after being recovered. According to the present invention, the method has characteristics of easy operation, high reaction yield, energy saving and environmental protection, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to the synthesis method of organic matter, in particular to a novel synthesis method of methyl heptanone. Background technique [0002] Methylheptanone, chemically named 6-methyl-heptan-2-one, is a colorless liquid with the aroma of lemongrass and butyl acetate. It has a strong chemical reaction ability and can be derived from a variety of products . It is an important intermediate in the synthesis of medicines, flavors and fragrances, and has a very high potential for commercial development. [0003] German patent DE1259876 and U.S. patent US3574773 disclose a kind of method that takes isobutylene as starting material, reacts with formaldehyde and acetone to synthesize methyl heptanone, the disadvantage of this method is that there are many side reactions, and by high temperature and high pressure reaction, the reaction conditions are relatively Harsh, not suitable for industrial production. [0004] U.S. Patents US398...

Claims

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Application Information

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IPC IPC(8): C07C45/73C07C49/04B01J31/28B01J31/02
CPCC07C45/73B01J23/44B01J31/0237B01J31/28B01J2231/4205B01J35/19C07C49/04
Inventor 黄升赵新颖
Owner JILIN BEISHA PHARMA
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