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Preparation method of cinnamaldehyde diethylacetal

A technology of cinnamaldehyde diethyl acetal and diethoxyethane, which is applied in the field of preparation of cinnamaldehyde diethyl acetal, can solve the problems of unsuitability for industrial production, low yield, easy hydrolysis, etc., and achieve easy removal , cost reduction, less side effects

Inactive Publication Date: 2012-10-03
湖北远成赛创科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The price of the raw material cinnamaldehyde used in this method is very high, and triethyl orthoformate is easily hydrolyzed; moreover, acetal reaction is a reversible reaction, when the reaction reaches equilibrium, it is difficult to continue; the general yield is not high, and it is not suitable for industrial production

Method used

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  • Preparation method of cinnamaldehyde diethylacetal
  • Preparation method of cinnamaldehyde diethylacetal
  • Preparation method of cinnamaldehyde diethylacetal

Examples

Experimental program
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Embodiment 1

[0020] Add 10g of triphenylphosphine, 101.5g of toluene, 0.4mol of benzaldehyde (M=106) and 0.3mol of 2-bromo-1,1-diethoxyethane (M=197) into a flat-bottomed flask and mix thoroughly Then pour it into a tubular reactor equipped with a macroporous resin carrier loaded with NaOH, put it into a microwave oven, and install a thermometer and a condenser. Microwave irradiation was carried out under the state of stirring and normal pressure, the power was 600W, the temperature was raised to 85°C, and the temperature was kept at reflux for 1.5h. After the reaction is completed, cool to room temperature after the reaction to obtain a reaction liquid, then distill off the solvent toluene under normal pressure, filter out the catalyst triphenylphosphine, and then further distill the reaction liquid through a scraper type molecular distillation device to obtain the product cinnamaldehyde diethyl acetal. The purity of the product is 99%, and the yield is 92.8%.

example 2

[0022] Add 10g of triphenylphosphine, 111g of toluene, 0.4mol of benzaldehyde and 0.35mol of 2-bromo-1,1-diethoxyethane into a flat-bottomed flask, mix well and pour into a macroporous resin loaded with KOH Carrier tube reactor, put it into a microwave oven, and install a thermometer and a condenser. Microwave irradiation was carried out under the state of stirring and normal pressure, the power was 550W, the temperature was raised to 88°C, and the temperature was kept at reflux for 1.5h. After the reaction is completed, cool to room temperature after the reaction to obtain a reaction liquid, then distill off the solvent toluene under normal pressure, filter out the catalyst triphenylphosphine, and then further distill the reaction liquid through a scraper type molecular distillation device to obtain the product cinnamaldehyde diethyl acetal. The purity of the product is 99%, and the yield is 93.3%.

example 3

[0024] Add 10 g of triphenylphosphine, 117 g of toluene, 0.4 mol of benzaldehyde and 0.38 mol of 2-bromo-1,1-diethoxyethane into a flat-bottomed flask, mix well, and pour into a loaded K 2 CO 3 Put it into a tubular reactor with a macroporous resin carrier, put it in a microwave oven, and install a thermometer and a condenser. Microwave irradiation was carried out under the state of stirring and normal pressure, the power was 500W, the temperature was raised to 90°C, and the temperature was kept at reflux for 2h. After the reaction is completed, cool to room temperature after the reaction to obtain a reaction liquid, then distill off the solvent toluene under normal pressure, filter out the catalyst triphenylphosphine, and then further distill the reaction liquid through a scraper type molecular distillation device to obtain the product cinnamaldehyde diethyl acetal. The product purity is 99%, and the yield is 93%.

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Abstract

The invention provides a preparation method of cinnamaldehyde diethylacetal. The preparation method comprises the following steps: using 2-bromo-1, 1-diethoxy ethane and benzaldehyde as raw material; and, synthesizing cinnamaldehyde diethylacetal through microwave radiation by taking triphenylphosphine as catalyst and solid carrier, wherein the solid carrier is alkaline macroporous resin. According to the preparation method, raw materials are cheap and easy to obtain, solid catalyst can be removed easily, the reaction condition is soft and simple, side reaction is less, the post-treatment is easy, the product yield and purity is high, the cost is greatly reduced, and the continuous production can be carried out.

Description

technical field [0001] The invention relates to the technical field of synthesis of fine chemical intermediates, in particular to a preparation method of cinnamaldehyde diethyl acetal. Background technique [0002] Cinnamaldehyde diethyl acetal, also known as cinnamaldehyde diethyl acetal, is a colorless transparent liquid with a similar aroma to cinnamaldehyde, but the aroma is softer and more natural. Cinnamaldehyde diethyl acetal can be used as flower-scented soap, head fragrance and modifier of detergent essence; it can also be used in citrus-type food flavor, which is allowed to be used in my country (GB2760-96). As a flavoring spice, the application amount in the seasoning is as high as 130ppm. [0003] The classic way of synthesizing cinnamaldehyde diethyl acetal is to obtain it through condensation of cinnamaldehyde and triethyl orthoformate or ethanol under the catalysis of inorganic liquid acid or Lewis acid. The price of the raw material cinnamaldehyde used in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/303C07C41/48C07C41/58
Inventor 叶思朱如慧杨洁韩洪杰徐海林
Owner 湖北远成赛创科技有限公司
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