Check patentability & draft patents in minutes with Patsnap Eureka AI!

Preparation method for alpha-amyl cinnamic aldehyde dimethyl acetal

A technology of cinnamaldehyde dimethyl acetal and pentyl cinnamaldehyde, which is applied in the field of fine chemical synthesis, can solve problems such as complicated processing procedures, affecting product quality, and deep product color, and achieves the advantages of improved purity, easy purification, and long-lasting aroma Effect

Inactive Publication Date: 2014-03-12
ANHUI HYEA AROMAS
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional synthesis method of α-pentyl cinnamaldehyde dimethyl acetal is composed of α-amyl cinnamaldehyde and anhydrous methanol in HCl or H 2 SO 4 It is prepared by condensation under catalysis, using concentrated acid as a catalyst. Because the concentrated acid corrodes the production equipment, it needs to carry out alkali washing and water washing processes. Darker, affecting product quality and reducing yield

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
  • Preparation method for alpha-amyl cinnamic aldehyde dimethyl acetal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] a) Use vacuum suction device 1 to add 200kg of α-amylcinnamaldehyde and 10kg of water-carrying cyclohexane into the 500L enamel reaction kettle 3. After the feeding is completed, replace the vacuum with nitrogen gas and add from the high tank 2 Methanol 80kg, add catalyst silica gel loaded zirconium sulfate 10kg from the hand hole of the reaction kettle, start the mixer and mix evenly;

[0021] b) Open the steam valve, heat up the enamel reaction kettle 3, and control the reaction temperature to 85~90°C;

[0022] c) After a reaction time of 4 hours, take a sample for gas chromatography detection, and when the content of α-amylcinnamaldehyde is less than 2%, cool down to terminate the reaction;

[0023] d) After the reaction is over, add 75kg of water to wash with water, and after standing for 2 hours, separate the lower layer of water through the observation of the mirror;

[0024] e) Transfer the upper oil layer of the reaction product in the enamel reaction kettle 3 ...

Embodiment 2

[0027] a) Add 240kg of α-amylcinnamic aldehyde and 12kg of water-containing cyclohexane to the 500L enamel reaction kettle by vacuum suction. After the feeding is completed, replace the vacuum with nitrogen, and add 100kg of methanol from the high-level tank , add 12 kg of ferric sulfate loaded on catalyst silica gel from the hand hole of the reaction kettle, start the mixer and mix evenly;

[0028] b) Open the steam valve, heat up the reactor, and control the reaction temperature to 85~90°C;

[0029] c) After a reaction time of 4 hours, take a sample for gas chromatography detection, and when the content of α-amylcinnamaldehyde is less than 2%, cool down to terminate the reaction;

[0030] d) After the reaction, add 80 kg of water, wash with water, let stand for 2 hours, and separate the lower layer of water through the observation mirror;

[0031] e) Transfer the upper oil layer of the reaction product in step d) to the fractionation still, raise the temperature of the stil...

Embodiment 3

[0034] a) Add 1,200kg of α-amylcinnamaldehyde and 60kg of water-containing cyclohexane to the 2500L enamel reaction kettle by vacuum suction. After the feeding is completed, replace the vacuum with nitrogen, and add 500kg of methanol from the high-level tank , add 55 kg of ferric sulfate loaded on catalyst silica gel from the hand hole of the reaction kettle, start the mixer and mix evenly;

[0035] b) Open the steam valve, heat up the reactor, and control the reaction temperature to 85~90°C;

[0036] c) After a reaction time of 4 hours, take a sample for gas chromatography detection, and when the content of α-amylcinnamaldehyde is less than 2%, cool down to terminate the reaction;

[0037] d) After the reaction is over, add 300kg of water to wash with water, and after standing for 2 hours, separate the lower layer of water through observation through the mirror;

[0038] e) Transfer the upper oil layer of the reaction product in step d) to the fractionating still, raise the ...

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

PropertyMeasurementUnit
refractive indexaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method for alpha-amyl cinnamic aldehyde dimethyl acetal. The preparation method comprises the following steps: adding alpha-amyl cinnamaldehyde and cyclohexane water-carrying agent to a reaction kettle in a vacuum intake manner; feeding nitrogen to displace vacuum; adding methanol and a catalyst; controlling the temperature of the reaction kettle to be 80-120 DEG C; 4 hours after the reaction, washing; layering by standing; transferring the upper oil layer of the reaction product to a fractionation kettle; recycling methanol which does not react at the normal pressure; under the condition that the pressure is 1000-3000 Pa, the temperature of the reaction kettle is 150-180 DEG C, and the reflux ratio is (2:1)-(1:10), fractionating out a crude alpha-amyl cinnamic aldehyde dimethyl acetal product. According to the invention, the alpha-amyl cinnamic aldehyde dimethyl acetal is synthetized in one step; the reaction conditions are mild; the purification treatment of the product is easy; the phenomena of equipment corrosion and generation of a great amount of waste acid liquid, caused when traditional concentrated acids such as sulfuric acid and hydrochloric acid are used as catalysts, are avoided; the purity of the end product reaches above 97%; the product has lasting fragrance, and is pure and mild.

Description

technical field [0001] The invention relates to a preparation method of organic synthetic spices in the technical field of fine chemical synthesis, in particular to a preparation method of α-pentyl cinnamaldehyde dimethyl acetal. Background technique [0002] α-Amylcinnamaldehyde dimethyl acetal, 2-(dimethoxymethyl)-1-heptenylbenzene, CAS No. 91-87-2, relative density (25°C) 0.955, refractive index (20°C) 1.508, insoluble in water, almost soluble in ethanol and propylene glycol, boiling point 300°C, flash point 92°C, colorless to light yellow oily liquid with soft fresh flower aroma. α-Amylcinnamic aldehyde dimethyl acetal can be used in daily chemical fragrance formulations, and is a good product for preparing jasmine fragrance series cosmetic fragrances. Its chemical properties are more stable than α-amylcinnamic aldehyde in alkaline medium, and it is not easy to be oxidized, so it is very suitable for soap flavor formulations, the dosage can reach 10%, and it has the adv...

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): C07C43/303C07C41/56
CPCC07C41/56C07C43/303
Inventor 王天义范一义汪民富董金龙
Owner ANHUI HYEA AROMAS
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com