Synthetic method of epsilon-decalactone perfume

A synthesis method and technology of decanolide, applied in directions such as organic chemistry, can solve the problems of complicated operation, high cost, harsh reaction conditions, etc., achieve high reaction yield and reduce the effect of separation and purification procedures

Inactive Publication Date: 2019-05-03
安徽华业香料合肥有限公司
View PDF5 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing ε-decalactone synthesis method has the disadvantages of high cost, harsh reaction conditions, complicated operation and low 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
  • Synthetic method of epsilon-decalactone perfume

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0031] For this reason, the inventor of the present invention provides a kind of synthetic method of ε-decalactone perfume, comprises the following steps:

[0032] (1) Mix the alkaline solution and part of cyclohexanone uniformly under the condition of heating and stirring to obtain mixture A; then add dropwise the mixture B of n-butyraldehyde and the remaining amount of cyclohexanone to the mixture A, after the addition is completed, Continue to stir and insulate and react until the content of n-butyraldehyde in the reactant is lower than 1.0%;

[0033] (2) The reactant of step (1) is left to stand, and the water layer is collected for recycling; the oil layer is collected, and the oil layer is washed to neutrality, and then the layers are left to stand, and the oil layer is collected to obtain the condensation product 2-butenyl cyclohexanone Crude;

[0034] (3) Utilize the rotary evaporator to distill the 2-butenyl cyclohexanone crude product, reclaim the cyclohexanone and ...

Embodiment 1

[0063] A kind of synthetic method of ε-decalactone perfume:

[0064] S1: In a 1000mL three-necked flask equipped with a thermometer, a stirrer, and a peristaltic pump, add 500mL of sodium hydroxide solution with a mass fraction of 2.5%, turn on the agitator and a constant temperature water tank, then add 50g of cyclohexanone, and mix well to obtain a mixture A; heat up to 75°C, dropwise add a mixture B of 40g of n-butyraldehyde and 60g of cyclohexanone to a three-necked flask through a peristaltic pump to carry out aldol condensation reaction, stir while adding, dropwise is completed after 3h, and then continue to stir to make The above reactants were kept warm for 2 hours at 75°C, and the reaction was terminated when the n-butyraldehyde content in the reactants was detected to be lower than 1%.

[0065] S2: Lower the temperature, transfer the reactant to a separatory funnel and let it stand for stratification for 2 hours; collect the sodium hydroxide solution in the water lay...

Embodiment 2

[0075] A kind of synthetic method of ε-decalactone perfume:

[0076] S1: In a 500mL three-neck flask equipped with a thermometer, a stirrer, and a peristaltic pump, add 250mL of sodium hydroxide solution with a mass fraction of 2.5%, turn on the agitator and a constant temperature water tank, then add 30g of cyclohexanone, and mix well to obtain a mixture A; heat up to 80°C, drop a mixture B of 15g of n-butyraldehyde and 30g of cyclohexanone into a three-necked flask through a peristaltic pump to carry out aldol condensation reaction, adopt drop-adding and stirring technology, stir while dropping, and finish adding in 2 hours , and then continue to stir, so that the above reactants are kept warm for 2 hours at 80° C., and the reaction is terminated when the n-butyraldehyde content in the reactants is lower than 1%;

[0077] S2: Cool down to normal temperature, transfer the reactant to the separatory funnel and let it stand for stratification for 2 hours; collect the sodium hyd...

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
quality scoreaaaaaaaaaa
quality scoreaaaaaaaaaa
purityaaaaaaaaaa
Login to view more

Abstract

The invention belongs to the technical field of perfume synthesis, and particularly relates to a synthetic method of epsilon-decalactone perfume. The synthetic method comprises the following steps: (1) mixing an alkaline solution with a part of cyclohexanone, then dropwise adding a mixture of n-butyraldehyde and the rest of cyclohexanone into the mixture, carrying out stirring, and carrying out heat preservation for a reaction; (2) standing the reactants in the step (1), collecting a water layer, collecting an oil layer, and washing the oil layer with water to obtain a condensed product 2-butenyl cyclohexanone crude product; (3) carrying out distilling to recover cyclohexanone to obtain 2-butenyl cyclohexanone; (4) carrying out a hydrogenation reaction; (5) collecting a liquid-phase intermediate product 2-butyl cyclohexanone crude product, and carrying out distilling to obtain 2-butyl cyclohexanone; (6) carrying out an oxidation reaction; and (7) carrying out distilling purification toobtain the epsilon-decalactone perfume product. According to the invention, the cyclohexanone is added into the reaction system in different ways, the excess cyclohexanone is used as a reaction solvent through a stirring dripping technology, and the cyclohexanone is reused after being recycled, so that separation and purification processes of the reaction solvent are reduced, and a high reactionyield is ensured.

Description

technical field [0001] The invention belongs to the technical field of perfume synthesis, and in particular relates to a synthesis method of ε-decalactone perfume. Background technique [0002] ε-decalactone is a colorless to pale yellow liquid with a sweet creamy aroma, which can be used in food flavors and has been approved by the American Flavor and Extract Manufacturers Association (FEMA No.3613) and approved by the FDA. edible. ε-decalactone is widely used in milk, cream essence and baked goods. However, the existing ε-decalactone synthesis method has the disadvantages of high cost, harsh reaction conditions, complicated operation and low yield. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a low-cost, high-yield and simple-to-operate synthetic method for ε-decalactone fragrance. [0004] In order to achieve the above object, the present invention adopts the following technical s...

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): C07D313/04
Inventor 王天义范一义徐基龙严四五
Owner 安徽华业香料合肥有限公司
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