Method for preparing trans3-heptylene-2-ketone

A technology of heptene and acetone, applied in the field of organic compound preparation, can solve the problems of complicated process and high preparation cost, and achieve the effects of stable process, low cost and no industrial wastes

Inactive Publication Date: 2015-06-03
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims at the problems existing in the above-mentioned prior art, and provides a method for preparing trans-3-hepten-2-one, which solves the problems of complicated process and high preparation cost in the prior art, and has no pollution to the environment

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing trans3-heptylene-2-ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 7.2g of n-butyraldehyde, 72g of triethylamine sulfate, 7.2g of calcium oxide, and 58g of acetone into the reaction flask, and place it under 200W microwave for TLC tracking until the reaction is complete, which takes about 20 minutes. After the reaction is complete, add 50ml of ethyl acetate, stir and let it stand, divided into upper and lower layers, the upper layer is the ethyl acetate solution of trans-3-hepten-2-one, the lower layer is solid alkali and ionic liquid; the lower layer is acetone Wash, remove acetone, heat the separated solid base and ionic liquid mixture to 60°C, and then dry it under vacuum for 12 hours to obtain the purified solid base and ionic liquid, which can be reused ; The upper liquid was rectified under the conditions of 15mmHg and 65-68°C to obtain 78 grams of trans-3-hepten-2-one, with a yield of 70%.

Embodiment 2

[0025] Add 7.2g of n-butyraldehyde, 72g of diethylamine sulfate, 15g of magnesium oxide, and 108g of acetone into the reaction flask, and place it under 500W microwave for TLC tracking until the reaction is complete, which takes about 10 minutes. After the reaction is complete, add 50ml of ethyl acetate, stir and let it stand, and divide it into upper and lower layers, the upper layer is the ethyl acetate solution of trans-3-hepten-2-one, and the lower layer is solid alkali and ionic liquid;

[0026] The lower layer is washed with acetone to remove acetone, the separated solid base and ionic liquid mixture is heated to 60°C, and then dried under vacuum for 12 hours to obtain the purified solid base and ionic liquid, and the purified solid base and ionic liquid Reusable; the upper liquid is rectified at 15mmHg, 65-68°C,

[0027] 70 g of trans-3-hepten-2-one can be obtained with a yield of 62.5%.

Embodiment 3

[0029] Add 7.2g of n-butyraldehyde, 72g of trimethylamine sulfate, 10g of magnesium oxide, and 108g of acetone into the reaction flask, and place it under 500W microwave for TLC tracking until the reaction is complete, which takes about 15 minutes. After the reaction is complete, add 50ml of ethyl acetate, stir and let it stand, and divide it into upper and lower layers, the upper layer is the ethyl acetate solution of trans-3-hepten-2-one, and the lower layer is solid alkali and ionic liquid;

[0030] The lower layer is washed with acetone to remove acetone, the separated solid base and ionic liquid mixture is heated to 60°C, and then dried under vacuum for 12 hours to obtain the purified solid base and ionic liquid, and the purified solid base and ionic liquid Reusable; the upper liquid is rectified at 15mmHg, 65-68°C,

[0031] 74 g of trans-3-hepten-2-one can be obtained with a yield of 66.1%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a method for preparing trans3-heptylene-2-ketone. The method comprises the following steps of: adding n-butanal, acetone, ionic liquid and solid alkali into a reaction bottle; under the action of microwave, after the reaction is complete, adding ethyl acetate, separating out lower-layer solid alkali and the ionic liquid which can be repeatedly utilized after being treated, separating out upper-layer liquid, carrying out distillation and obtaining the trans3-heptylene-2-ketone. The method is low in cost, stable in process and easy in recycling catalysts and solvents, has no three industrial wastes and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation; in particular, it relates to a method for preparing trans-3-hepten-2-one. Background technique [0002] Trans-3-hepten-2-one widely exists in plants in nature, has a strong grass smell, is recognized as safe, and is an important spice additive, widely used in the food industry, in GB2760-86 standard It is specified as a food spice that is allowed to be used. There are three main methods for its synthesis. (See literature; 1, Li Wei, Liu Yun, Journal of Beijing Technology and Business University, 2001.19 (4). 13-15. 2, patent FR2481701. 3, patent JP7424456). The first method is obtained by condensing n-butyraldehyde and acetone under the action of alkali. The second method is obtained by the acylation reaction of acid chlorides and alkenes under acid catalysis. The third method is obtained by reacting 2-hexenoic acid with methyllithium. Wherein the first method is the che...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/74
CPCC07C45/74C07C49/203
Inventor 陈平兰鲲
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap