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Method for preparing 2-ethyl-4-(2,2,3-trimethylcyclopent-3-en-yl)-but-2-enal

A technology of borneolenyl butyraldehyde and borneolenal, which is applied in the field of preparation of 2-borneolenyl butyraldehyde, can solve the difficulty in aroma processing of sandalwood products, low equipment utilization rate, and low conversion rate. Advanced problems, to achieve the effect of improved product quality, mild reaction conditions, and simple aroma treatment

Inactive Publication Date: 2013-06-05
杭州友邦香料香精有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of 2-borneolenyl butyraldehyde is to utilize borneolenal and n-butyraldehyde as raw material, sodium hydroxide or potassium hydroxide is a catalyst, and methyl alcohol is synthesized as a solvent, but such synthetic method equipment utilization rate is not enough High, low conversion rate, and many side reactions, it is difficult to process the aroma of sandalwood products used for synthesis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Add 225g of borneolenal and 26g of morpholine into a 1000ml four-necked flask (equipped with stirring, thermometer, reflux condenser, and dropping funnel), stir and heat up to 65-90°C, prepare 250g of n-butyraldehyde, acetic acid 45g, then add n-butyraldehyde and acetic acid respectively in order: add 25g n-butyraldehyde (10% of the total amount of n-butyraldehyde) dropwise for the first time, control the temperature at 65-90°C, and then add 14.85g of acetic acid (10% of the total amount of acetic acid) 33%), the temperature is controlled at 70-95°C; the temperature of the second to seventh addition of n-butyraldehyde and the addition of acetic acid are all controlled at 70-95°C, and the second drop-wise addition of n-butyraldehyde is 27.5% of the total amount of n-butyraldehyde, Then drop into 32% of the total amount of acetic acid; drop 27.5% of the total amount of n-butyraldehyde for the third time, then drop into 8.75% of the total amount of acetic acid; ...

Embodiment 2

[0021] Example 2: Add 250g of borneolenal and 35g of morpholine into a 1000ml four-neck flask (equipped with stirring, thermometer, reflux condenser, and dropping funnel), stir and heat up to 65-90°C, prepare 280g of n-butyraldehyde, acetic acid 65g, then add n-butyraldehyde and acetic acid respectively in order: add 28g n-butyraldehyde (10% of the total amount of n-butyraldehyde) dropwise for the first time, control the temperature at 65-90°C, and then add 21.45g of acetic acid (10% of the total amount of acetic acid) 33%), the temperature is controlled at 70-95°C; the temperature of the second to seventh addition of n-butyraldehyde and the addition of acetic acid are all controlled at 70-95°C, and the second drop-wise addition of n-butyraldehyde is 27.5% of the total amount of n-butyraldehyde, Then drop into 32% of the total amount of acetic acid; drop 27.5% of the total amount of n-butyraldehyde for the third time, then drop into 8.75% of the total amount of acetic acid; 10...

Embodiment 3

[0022] Example 3: The difference from Example 1 is that the catalyst I was changed from morpholine to piperidine to obtain the finished product of 2-bornylidene butyraldehyde with a content of 94% and a yield of 91.8%.

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PUM

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Abstract

The invention relates to a method for preparing 2-ethyl-4-(2,2,3-trimethylcyclopent-3-en-yl)-but-2-enal, which comprises the following steps: synthesizing the 2-ethyl-4-(2,2,3-trimethylcyclopent-3-en-yl)-but-2-enal by campholenic aldehyde and n-butanal which are taken as raw materials, putting the campholenic aldehyde and a catalyst I into a reaction kettle, and heating to the temperature of between 65 and 90 DEG C, wherein the mass ratio of the campholenic aldehyde to the catalyst I is 1:0.1-0.2; orderly adding the n-butanal and a catalyst II into the mixed solution of the campholenic aldehyde and the catalyst I respectively, wherein the mass ratio of the campholenic aldehyde to the n-butanal is 1:1.0-1.5, and the mass ratio of the campholenic aldehyde to the catalyst II is 1:0.1-0.4; and after addition of the materials, controlling the temperature to between 75 and 100 DEG C, continuously reacting for 2 to 3 hours, washing crude product oil with water to neutrality, and distilling the crude product oil under reduced pressure to obtain the 2-ethyl-4-(2,2,3-trimethylcyclopent-3-en-yl)-but-2-enal. The method has the advantages that: the campholenic aldehyde and n-butanal are adopted as main raw materials to synthesize the 2-ethyl-4-(2,2,3-trimethylcyclopent-3-en-yl)-but-2-enal product, the reaction conditions are mild, the operation is safe and convenient, the yield and qualityof the product are greatly improved, and the aroma of sandalwood products synthesized is simple to treat.

Description

technical field [0001] The invention relates to a chemical synthesis method in the field of fragrances, and mainly relates to a preparation method of 2-bornylidene butyraldehyde. Background technique [0002] 2-bornylidene butyraldehyde is an important intermediate product in the synthesis of fragrance 2-bornylidene butanol, which is called Sandalwood 208 in my country. It has a strong sandalwood aroma and a faint rose fragrance, and the fragrance lasts for a shorter time than natural sandalwood oil. Widely used in soap, cosmetics, shampoo and other daily chemical essence formulations. The preparation method of 2-borneolenyl butyraldehyde is to utilize borneolenal and n-butyraldehyde as raw material, sodium hydroxide or potassium hydroxide is a catalyst, and methyl alcohol is synthesized as a solvent, but such synthetic method equipment utilization rate is not enough High, low conversion rate, and many side reactions, it is difficult to process the aroma of sandalwood prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/225C07C45/74B01J31/02B01J31/04
Inventor 王利人翁卫栋王璟琳
Owner 杭州友邦香料香精有限公司