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Preparation method of cis-3-hexenal

A technology of dilute aldehyde and hexenol, which is applied in the field of preparation of cis-3-hexenaldehyde, can solve problems such as difficult separation and dispersion, and achieve the effects of low equipment requirements, simplified preparation process, and easy cost

Inactive Publication Date: 2013-08-14
TIANNING FLAVOR JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the fragrance and its alcohols widely exist in nature, because they are relatively dispersed and difficult to separate, the problem of how to artificially synthesize it has attracted the attention of many foreign fragrance companies and organic chemists.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Synthesis of catalyst-refined IBX: In a 250ml three-necked flask equipped with a stirring and spherical condenser, dissolve 0.06mol potassium hydrogen persulfate reagent into 9mol deionized water, and then add 0.04mol o-iodobenzoic acid at one time. The mixed liquid was heated to 75°C in 20 minutes and stirred at this temperature for 2 hours. After the reaction was completed, the suspension was cooled to 5°C with ice water and stirred at this temperature for 1 hour. The mixture was filtered, washed with 6*100ml of deionized water and 2*100ml of acetone, respectively, to obtain 10.08g of IBX crystals with a yield of 90%. The obtained IBX crystals were dissolved in 120 ml of 75% ethanol and recrystallized 5 times. Finally, it was filtered, washed and dried to obtain 9.072 g of purified IBX white crystals with a melting point of 231°C. The yield is 90%.

[0014] Synthesis of cis-3-hexenal: In a 250ml three-necked flask equipped with a stirring and spherical condenser, ad...

Embodiment 2

[0016] Synthesis of catalyst-refined IBX: In a 250ml three-necked flask equipped with a stirring, spherical condenser, dissolve 0.06 mol of potassium hydrogen persulfate reagent into 9 mol of deionized water, and then add 0.04 mol of o-iodobenzoic acid at one time. The mixed liquid was heated to 73°C in 15 minutes and stirred at this temperature for 3 hours. After the reaction was completed, the suspension was cooled to 2°C with ice water and stirred at this temperature for 1.5 hours. The mixture was filtered and washed with 8*100ml of deionized water and 5*100ml of acetone, respectively, to obtain 10.30 g of IBX crystals with a yield of 92%. The obtained IBX crystals were dissolved in 120 ml of 80% ethanol and recrystallized 8 times. Finally, it was filtered, washed and dried to obtain 9.27 g of purified IBX white crystals with a melting point of 231°C. The yield is 90%.

[0017] Synthesis of cis-3-hexenal: In a 250ml three-necked flask equipped with a stirring and spherica...

Embodiment 3

[0019] Catalyst-purified IBX synthesis: In a 250ml three-necked flask equipped with a stirring, spherical condenser, dissolve 0.025mol potassium hydrogen persulfate reagent into 4mol deionized water, and then add 0.015mol o-iodobenzoic acid at one time. The mixed liquid was heated to 75°C in 15 minutes and stirred at this temperature for 1 hour. After the reaction was completed, the suspension was cooled to 5°C with ice water and stirred at this temperature for 1 hour. The mixture was filtered and washed with 6*100ml of deionized water and 2*100ml of acetone, respectively, to obtain 3.65g of IBX crystals with a yield of 87%. The obtained IBX crystals were dissolved in 100 ml of 75% ethanol and recrystallized 5 times. Finally, it was filtered, washed and dried to obtain 3.32 g of purified IBX white crystals with a melting point of 231°C. The yield is 91%.

[0020] Synthesis of cis-3-hexenal: In a 250ml three-necked flask equipped with a stirring and spherical condenser, add 0...

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Abstract

The invention discloses a preparation method of cis-3-hexenal. By adopting DMSO (dimethyl sulfoxide) as a solvent and IBX as a catalyst, the method is used for preparing the cis-3-hexenal from a raw material cis-3-hexenol by a direct oxidation reaction. According to the preparation method disclosed by the invention, the adopted raw material has low cost and is easily available; the prepared product has high yield, and operation conditions are mild; and the preparation method has low requirements for the production equipment and is suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of cis-3-hexenaldehyde, in particular to a method for preparing cis-3-hexenaldehyde by using IBX as a catalyst. Background technique [0002] With the development of the national economy, people's life has gradually changed from subsistence to a well-off type, which provides a broad market for the development of spice industry products, especially natural spice is favored. However, because natural animal and plant spices are often limited by natural conditions and processing factors, the number of varieties and product quality are affected to a certain extent. (Resources are limited, coupled with the relatively small proportion contained in the organism, the yield is low, and the price remains high, which cannot meet the demand.) The innovation and quality improvement of flavors are also increasingly dependent on new synthetic flavors. Because synthetic fragrances are not limited by natural conditi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/29C07C47/21
Inventor 吴义龙张贡博张树林周春飞
Owner TIANNING FLAVOR JIANGSU
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