Preparation technology of alpha, alpha-dimethyl-ethide phenylpropyl aldehyde

A technology for the preparation of ethyl phenylpropionaldehyde, which is applied in the field of α, and can solve the problems of low yield, large pollution, and high cost of the preparation process

Inactive Publication Date: 2009-09-09
孙玉明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the synthetic method of α, α-dimethyl-ethyl-phenylpropionaldehyde (Chemical World 1988, VOL2, 9) is obtained by reacting ethylbenzene with isobutyraldehyde through chloromethylation, and the used Most of the catalysts are alkyl ammonium iodides. This preparation process has low yield, high cost and large pollution

Method used

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  • Preparation technology of alpha, alpha-dimethyl-ethide phenylpropyl aldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 20% sodium hydroxide solution, benzene, triethylamine, and sodium iodide in sequence in the reaction kettle, stir and heat up to 70°C, and add the mixture of ethylbenzyl chloride and isobutyraldehyde dropwise under this temperature condition, 5 Drop within 1 hour, keep warm for 2 hours, cool to room temperature, add water, stir, let stand for liquid separation, take the supernatant liquid and add phosphoric acid, heat to 70 degrees, stir for 1 hour, wash off the enol ether, then wash with water, dehydrate, and distill get the product.

Embodiment 2

[0022] Add 40% sodium hydroxide solution, toluene, triethylamine, and potassium iodide in sequence in the reaction kettle, stir, and raise the temperature to 70°C. Under this temperature condition, add the mixture of ethylbenzyl chloride and isobutyraldehyde dropwise, within 8 hours After dripping, keep warm for 3 hours, cool to room temperature, add water, stir, stand for liquid separation, take the supernatant liquid and add phosphoric acid, heat to 75 degrees, stir for 2 hours, wash off the enol ether, then wash with water, dehydrate, and distill to obtain the product .

Embodiment 3

[0024] Add 40% potassium hydroxide solution, xylene, tetrabutylammonium bromide, and potassium iodide in sequence in the reaction kettle, stir, raise the temperature to 75°C, and add the mixture of ethylbenzyl chloride and isobutyraldehyde dropwise under this temperature condition , drop it within 10 hours, keep warm for 3 hours, cool to room temperature, add water, stir, stand still and separate the liquid, take the upper layer and add p-toluenesulfonic acid, heat to 75 ° C, stir for 3 hours, wash off the enol ether, and then Washed, dehydrated, distilled products.

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Abstract

The invention discloses a preparation technology of alpha, alpha-dimethyl-ethide phenylpropyl aldehyde. The preparation technology is as follows: ethide benzyl chloride and isobutylaldehyde are taken as major raw materials, aromatic hydrocarbon is a solvent under the condition of alkalescence and is added with a catalytic agent, the aromatic hydrocarbon is stirred and heated under the temperature of 60-95 DEG C to be reacted, and then the aromatic hydrocarbon is washed by protonic acid water under the temperature of 50-95 DEG C to eliminate enol ether so as to obtain the alpha, alpha-dimethyl-ethide phenylpropyl aldehyde. The preparation technology not only has simple operation and reduces the environment pollution, but also has high yield coefficient of products; in addition, the content of the gas phase chromatography of obtained products is 80-95 percent.

Description

technical field [0001] The invention relates to the field of synthetic perfumes, in particular to a preparation process of α,α-dimethyl-ethylphenylpropionaldehyde. Background technique [0002] α,α-Dimethyl-ethylphenylpropionaldehyde, also known as sea breeze aldehyde, is an important spice with a fresh flowery fragrance of rabbit ears and a sea breeze-like rhyme. It is widely used in soaps, washing powder, cosmetics, etc. The product is in production. At present, the synthetic method of α, α-dimethyl-ethyl-phenylpropionaldehyde (Chemical World 1988, VOL2, 9) is obtained by reacting ethylbenzene with isobutyraldehyde through chloromethylation, and the used Most of the catalysts are alkyl ammonium iodides. This preparation process has low yield, high cost and heavy pollution. Contents of the invention [0003] The purpose of the present invention is to provide a kind of simple operation, high yield, little pollution α, α-dimethyl-ethylphenylpropanal preparation process fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/228C07C45/68B01J31/26B01J31/02
Inventor 孙玉明
Owner 孙玉明
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