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Preparation method of cinnamyl cinnamate

A technology of cinnamic acid and methyl laurate, which is applied in the field of preparation of cinnamic acid, can solve problems such as difficult crystallization, complex process, and many by-products, so as to avoid side reaction products, shorten reaction time, and improve conversion rate effect

Active Publication Date: 2018-04-06
YANCHENG CITY CHUNZHU AROMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2. Use hot caustic alkali solution to process natural styrax balsam and Peru balsam to extract cinnamon laurate. The cost of cinnamon laurate produced by this method is high, raw materials are difficult to find, the process is complicated, and it seriously pollutes the environment
This process has the problems of long reaction cycle, many by-products, difficult crystallization, serious pollution, and low yield.

Method used

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  • Preparation method of cinnamyl cinnamate
  • Preparation method of cinnamyl cinnamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Reaction

[0056] In an oil bath, 117.36g of methyl laurate, 194.40g of cinnamon and 8.58g of potassium carbonate were put into a 500ml three-necked flask, and the resulting mixture was heated to an internal temperature of 120°C under stirring, and methanol began to distill out. After 1 hour, the reaction temperature rose to 160°C and stopped heating, and cooled to 80°C to obtain a reaction solution containing cinnamic acid;

[0057] (2) Washing and recycling

[0058] Add 300g of ethyl acetate and 150g of water to the reaction solution containing cinnamic acid obtained in step (1), stir and separate layers, and after separating the water layer, continue to add 150g of water to the oil layer to wash to neutrality, separate the water layer, and heat to recover acetic acid Ethyl 264g, changed to vacuum distillation at a pressure of 0.1KPa and a temperature of 205°C, and a fraction of 207.6g was collected, which was the crude cinnamic acid ester;

[0059] (3) crystall...

Embodiment 2

[0063] (1) Reaction

[0064] In an oil bath, put 117.36g of methyl laurate, 194.40g of cinnamon alcohol and 5.87g of potassium carbonate into a 500ml three-necked flask, and the resulting mixture was heated to an internal temperature of 120°C under stirring, and methanol began to distill out. After 1.5 hours, the reaction temperature rose to 160°C and stopped heating, and cooled to 80°C to obtain a reaction solution containing cinnamic acid;

[0065] (2) Washing and recycling

[0066] Add 300g of ethyl acetate and 150g of water to the reaction solution containing cinnamic acid obtained in step (1), stir and separate layers, and after separating the water layer, continue to add 150g of water to the oil layer to wash to neutrality, separate the water layer, and heat to recover acetic acid Ethyl 264g, changed to vacuum distillation at a pressure of 0.2KPa and a temperature of 195-205°C, and a fraction of 187.6g was collected, which was the crude cinnamic acid ester;

[0067] (3...

Embodiment 3

[0071] (1) Reaction

[0072] In an oil bath, put 117.36g of methyl laurate, 234.72g of cinnamyl alcohol and 11.74g of potassium carbonate into a 500ml three-necked flask, and the resulting mixture was heated to an internal temperature of 120°C under stirring, and methanol began to distill out. After 3 hours, the reaction temperature rose to 160°C and stopped heating, and cooled to 80°C to obtain a reaction solution containing cinnamic acid;

[0073] (2) Washing and recycling

[0074] Add 350g of ethyl acetate and 180g of water to the reaction solution containing cinnamic acid obtained in step (1), stir and separate layers, and after the water layer is separated, the oil layer continues to be washed with 180g of water to neutrality, and the water layer is separated, and heating reclaims acetic acid Ethyl 284g, changed to vacuum distillation at a pressure of 0.2KPa and a temperature of 195-205°C, and a fraction of 157.6g was collected, which was the crude cinnamon laurate;

[...

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Abstract

The invention relates to a preparation method of cinnamyl cinnamate. In an oil bath, methyl cinanmate, cinnamyl alcohol and potassium carbonate are mixed and heated under stirring, and low boiling substances are distilled off while reacting, heating is stopped to cool, water and ethyl acetate are added for washing until the water phase is neutral, and the oil phase is subjected to reduced pressuredistillation after being heated to recover ethyl acetate so as to obtain cinnamyl cinnamate crude products, and the cinnamyl cinnamate crude products are recrystallized from ethanol to obtain white solid cinnamyl cinnamate. The preparation method has the advantages of simple process, short cycle, high yield, simple post-treatment, green environmental protection and the like. The cinnamyl cinnamate prepared according to the method has the advantages of pure aroma, good color, high purity and the like.

Description

【Technical field】 [0001] The invention belongs to the technical field of perfume synthesis. More specifically, the present invention relates to a kind of preparation method of cinnamon laurate. 【Background technique】 [0002] Cinnamyl cinnamate, chemical name phenylpropenyl acrylate, English name cinnamylcinnamate, alias cinnamyl cinnamate, naturally exists in balsams such as Suhe balsam and white Peru balsam, and has a floral balsam aroma. Cinnamyl laurate is an important fine chemical intermediate, widely used in the production of medicines, spices and other products, mainly used as a fixative in flavors, and can be used to blend carnation, hyacinth, tuberose, Floral essences such as heart orchid, sandalwood, white orchid, and lily of the valley are widely used in the fragrance, fragrance and cosmetics industry, and are also included in GB2760, and are allowed to be used as food additives. [0003] At present, there are several methods for preparing cinnamic acid: 1. It ...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C67/54C07C67/52C07C69/618
CPCC07C67/03C07C67/52C07C67/54C07C69/618
Inventor 王冠沈海燕吴兵
Owner YANCHENG CITY CHUNZHU AROMA
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