Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Refining method of high-purity trans-Alpha-methylcinnamaldehyde

A technology of methyl cinnamaldehyde and a refining method, which is applied in the field of fine chemical synthesis, can solve problems such as difficult separation and waste of resources, and achieve the effects of increasing yield, saving costs, and avoiding waste

Active Publication Date: 2015-11-25
YINGCHENG WUHAN ORGANIC MATERIAL CO LTD
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the problem of high content of cis-α-methylcinnamaldehyde in the existing trans-α-methylcinnamaldehyde synthesis process, which is difficult to separate, discards and wastes resources

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
  • Refining method of high-purity trans-Alpha-methylcinnamaldehyde
  • Refining method of high-purity trans-Alpha-methylcinnamaldehyde
  • Refining method of high-purity trans-Alpha-methylcinnamaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In order to overcome the problems of high content of cis-α-methylcinnamaldehyde in the existing trans-α-methylcinnamaldehyde synthesis process, which is difficult to separate, waste and waste resources, this embodiment provides a high-purity trans-α-methylcinnamaldehyde The refining method of methyl cinnamaldehyde,

[0018] 1) Preparation of the crude product of α-methylcinnamaldehyde; the crude product of α-methylcinnamaldehyde obtained by condensation, neutralization and desolvation of benzaldehyde and n-propionaldehyde, wherein the crude product of α-methylcinnamaldehyde includes benzene Formaldehyde, benzyl alcohol, cis-alpha-methylcinnamaldehyde, trans-alpha-methylcinnamaldehyde, and 2-methyl-3-hydroxy-3-phenylpropanal.

[0019] Wherein, the main reaction principle of benzaldehyde and n-propionaldehyde reaction is:

[0020]

[0021] The side reactions in this reaction are:

[0022]

[0023] 2) primary rectification; the α-methylcinnamaldehyde crude product ...

Embodiment 2

[0034] On the basis of Example 1, this example specifically provides a method for refining high-purity trans-α-methylcinnamaldehyde:

[0035] First, 500 grams of the dehydrated crude product of α-methylcinnamaldehyde crude product obtained by condensation of benzaldehyde and n-propionaldehyde is rectified and purified under vacuum-0.099MPa, wherein the composition of the dehydrated crude product of α-methylcinnamaldehyde crude product is trans Formula α-methylcinnamaldehyde 75%, cis-α-methylcinnamaldehyde 2.5%, benzaldehyde 18%, benzyl alcohol 1.5%, obtain 95 grams of low boiling components, 50 grams of transition fractions, 330 grams of finished products, high boiling 20 grams; Among them, the transitional fraction is divided into cis-α-methylcinnamaldehyde 10.5%, trans-α-methylcinnamaldehyde 87%; the finished product components are cis-α-methylcinnamaldehyde 3.5%, trans-α - Methylcinnamaldehyde 96.2%.

[0036] Then, 300 grams of the finished product obtained above were rect...

Embodiment 3

[0039] This embodiment specifically provides a method for refining high-purity trans-α-methylcinnamaldehyde:

[0040] First, 500 grams of the dehydrated crude product of α-methylcinnamaldehyde crude product obtained by condensation of benzaldehyde and n-propionaldehyde is rectified and purified under vacuum-0.099MPa, wherein the composition of the dehydrated crude product of α-methylcinnamaldehyde crude product is trans Formula α-methylcinnamaldehyde 75%, cis-α-methylcinnamaldehyde 2.5%, benzaldehyde 18%, benzyl alcohol 1.5%, obtain 95 grams of low boiling components, 50 grams of transition fractions, 330 grams of finished products, high boiling 20 grams; Among them, the transitional fraction is divided into cis-α-methylcinnamaldehyde 10.5%, trans-α-methylcinnamaldehyde 87%; the finished product components are cis-α-methylcinnamaldehyde 3.5%, trans-α - Methylcinnamaldehyde 96.2%.

[0041] Then, 300 grams of the finished product obtained above were rectified and purified under...

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 provides a refining method of high-purity trans-Alpha-methylcinnamaldehyde. The high-purity trans-Alpha-methylcinnamaldehyde higher than 99.0% in content is acquired by condensing benzaldehyde and propionaldehyde in solvent under the action of phase transfer catalyst to obtain crude Alpha-methylcinnamaldehyde and subjecting the crude Alpha-methylcinnamaldehyde to first rectification, second rectification, acid decomposition and third rectification. The yield of the high-purity trans-Alpha-methylcinnamaldehyde is increased.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a method for refining α-methylcinnamaldehyde. Background technique [0002] α-Methylcinnamaldehyde is a spice with a wide range of uses. It is often used in the fragrance of cosmetics, soaps, foods, etc. At the same time, α-Methylcinnamaldehyde is also an important intermediate of the diabetes drug Eparestein, and the commercial product is trans α-Methylcinnamaldehyde, with the increase of diabetic patients, the demand for this drug increases, and the demand for intermediates also increases. Therefore, it is necessary to improve its synthesis process to improve its quality. [0003] At present, the synthesis of α-methylcinnamaldehyde is formed by condensation of benzaldehyde and n-propionaldehyde in a solvent under the action of a phase transfer catalyst. A kind of, what is used for pharmaceutical intermediate is trans α-methyl cinnamaldehyde, yet, in...

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
IPC IPC(8): C07C47/232C07C45/82C07C45/67C07C45/74C07C45/78
CPCC07C45/67C07C45/74C07C45/78C07C45/82C07C47/232
Inventor 刘志辉
Owner YINGCHENG WUHAN ORGANIC MATERIAL CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com