Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of fragrance intermediate

A technology of intermediates and fragrances, applied in the field of flavors and fragrances, can solve the problems of unrecyclable utilization, catalyst pollution, low selectivity of n-methyl pseudoionone, etc., and achieve convenient post-processing, high conversion rate and high selectivity Effect

Active Publication Date: 2018-01-12
广东恒裕生物科技有限公司
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to overcome the technical problems of high catalyst pollution and inability to recycle, low selectivity of n-methyl pseudo-ionone in the preparation process of perfume intermediate n-methyl pseudo-ionone in the prior art, and provide a n-methyl pseudo-ionone The preparation method of base pseudo-ionone

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
  • A kind of preparation method of fragrance intermediate
  • A kind of preparation method of fragrance intermediate
  • A kind of preparation method of fragrance intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Preparation of catalyst:

[0037] Add 30g of alumina powder to the mixed solution of 300ml of DMF and water (the volume ratio of DMF and water is 5:1), and diffuse it sufficiently by ultrasonic at room temperature; add 2N sodium hydroxide aqueous solution dropwise at 40°C, Stir the reaction for 30 minutes; after adding the sodium hydroxide dropwise solution, immediately add 2-methylimidazole (among them aluminum oxide: sodium hydroxide: 2-methylimidazole = 1:0.8:2.0), and react 2- at 80-90°C Filtrate for 3 hours, wash, and dry at 55-65°C to obtain the precursor; put the precursor in a nitrogen atmosphere and heat up carbonization, the carbonization temperature is 200°C; then naturally cool to room temperature to obtain a specific surface area of ​​720 m 2 g -1 aza-modified alumina nanoparticles.

[0038] 2) Catalytic reaction

[0039] Add 100g of citral and the catalyst prepared above into the reactor and stir for 20-30 minutes; raise the temperature to 45-50°C, ...

Embodiment 2

[0041] 1) Preparation of catalyst:

[0042] Add 30g of alumina powder to the mixed solution of 300ml of DMF and water (the volume ratio of DMF and water is 5:1), and diffuse it sufficiently by ultrasonic at room temperature; add 2N sodium hydroxide aqueous solution dropwise at 40°C, Stir the reaction for 30 minutes; after adding the sodium hydroxide dropwise solution, immediately add 2-methylimidazole (among them aluminum oxide: sodium hydroxide: 2-methylimidazole = 1:1.5:2.0), and react 2- at 80-90°C Filtrate for 3 hours, wash, and dry at 55-65°C to obtain the precursor; put the precursor in a nitrogen atmosphere and heat up carbonization, the carbonization temperature is 450°C; then naturally cool to room temperature to obtain a specific surface area of ​​810m 2 g -1 aza-modified alumina nanoparticles.

[0043] 2) Catalytic reaction

[0044] Add 100g of citral and the catalyst prepared above into the reactor and stir for 20-30min; heat up to 45-50°C, add butanone dropwis...

Embodiment 3

[0046] 1) Preparation of catalyst:

[0047]Add 30g of alumina powder to the mixed solution of 300ml of DMF and water (the volume ratio of DMF and water is 5:1), and diffuse it sufficiently by ultrasonic at room temperature; add 2N sodium hydroxide aqueous solution dropwise at 40°C, Stir the reaction for 30 minutes; after adding the sodium hydroxide dropwise solution, immediately add 2-methylimidazole (among them aluminum oxide: sodium hydroxide: 2-methylimidazole = 1 : 1.2 : 2.3), and react 2- at 80-90°C Filtrate for 3 hours, wash, and dry at 55-65°C to obtain the precursor; put the precursor in a nitrogen atmosphere and heat up carbonization, the carbonization temperature is 200°C; then naturally cool to room temperature to obtain a specific surface area of ​​860 m 2 g -1 aza-modified alumina nanoparticles.

[0048] 2) Catalytic reaction

[0049] Add 100g of citral and the catalyst prepared above into the reactor and stir for 20-30min; heat up to 45-50°C, add butanone dro...

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 belongs to the technical field of flavors and fragrances, and specifically relates to a preparation method of fragrance intermediates. The present invention uses aza-modified aluminum oxide nanosphere particles as catalysts to catalyze the reaction of citral and butanone to generate methyl pseudoionone, and the selectivity of n-methyl pseudoionone among the methyl pseudoionone is high. The present invention has high catalytic efficiency, high conversion rate of citral, and high selectivity of n-methyl pseudoionone, in which the selectivity of n-methyl pseudoionone and isomethyl pseudoionone is greater than 25:1; in addition; The catalyst of the invention can be recycled and reused without affecting the selectivity of the product and the conversion rate of the substrate.

Description

technical field [0001] The invention belongs to the technical field of flavors and fragrances, and in particular relates to a method for preparing a fragrance intermediate. Background technique [0002] Methyl ionone is a homologue of ionone, but its aroma grade is better than ionone. Its beautiful and soft fragrance and good stability are favored by people. N-methyl pseudoionone is a widely used intermediate in the perfume synthesis industry. It is an indispensable raw material for the synthesis of n-methyl ionone, and its content directly affects the content of n-methyl ionone in the later stage. The level of the level and the charm of the overall aroma. [0003] Ionone is produced by pseudo-ionone, which is usually produced by aldol condensation of citral and acetone under alkaline conditions. The reaction formula is as follows (1): [0004] [0005] (1) [0006] N-methyl ionone is synthesized from n-methyl pseudoionone, which is produced by aldol condensation of ci...

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 Patents(China)
IPC IPC(8): C07C45/74C07C49/203B01J27/24B01J35/08B01J35/10
CPCC07C45/74B01J27/24B01J35/51B01J35/617C07C49/203Y02P20/584
Inventor 邓伟战
Owner 广东恒裕生物科技有限公司