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Method for preparing linalyl acetate by linalool and acetic anhydride

A technology of linalyl acetate and acetic anhydride, which is applied in the field of preparing linalyl acetate from linalool and acetic anhydride, which can solve the difficult separation and recovery of products, increase the production cost of linalyl acetate, low yield of linalyl acetate, etc. question

Inactive Publication Date: 2005-01-19
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because linalool is an allyl tertiary alcohol, it is unstable in the presence of protonic acid, and isomerization, cyclization and elimination reactions easily occur, generating a large amount of by-products, resulting in a very low yield of linalyl acetate, generally only Can reach 40%
Relatively speaking, the yield of linalyl acetate is higher by using a basic catalyst such as dimethylaminopyridine, but this basic catalyst is dissolved in the reaction solution, and it is difficult to separate and recover from the product, which not only increases the yield of linalyl acetate. Production costs, but also affect the quality of the product

Method used

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  • Method for preparing linalyl acetate by linalool and acetic anhydride
  • Method for preparing linalyl acetate by linalool and acetic anhydride
  • Method for preparing linalyl acetate by linalool and acetic anhydride

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Experimental program
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Effect test

Embodiment 1

[0017] Catalyst preparation:

[0018] In a 250ml three-necked flask placed on an oil bath, add 0.6g melamine and 18g methyl p-toluenesulfonate, 0.2g NaOH as a catalyst and 10ml toluene as a solvent, stir and raise the temperature to 80°C and maintain it for 6 hours. Then perform hot filtration, wash the filter cake with acetone after cooling, and dry under vacuum at room temperature to obtain the finished catalyst.

[0019] The intensity of characteristic resonant peak of the methyl group was measured by infrared spectroscopy on the catalyst, and the degree of methylation of the methyl-modified melamine was estimated to be 45%.

[0020] Preparation of linalyl acetate:

[0021] Put 33.5g of linalool and 30g of acetic anhydride into a 250ml three-necked flask, add 0.02g of the catalyst obtained above, stir and heat up to 80°C, keep it standing for cooling after 6 hours, remove the catalyst by filtration, and obtain the composition of each component through gas chromatography an...

Embodiment 2～4

[0023] During the preparation of the catalyst, the methylation reaction time of melamine and methyl p-toluenesulfonate was changed to 5, 5.5, and 6.5 hours, respectively, and the methylation degree was 35%, 41%, and 55% respectively. Melamine is as catalyzer, and all the other are with embodiment 1.

Embodiment 5～7

[0025] The preparation of catalyst is with embodiment 1, changes the consumption of catalyst during esterification, all the other are with embodiment 1.

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PUM

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Abstract

The invention discloses a process for preparing linalyl acetate from linalool and acetic anhydride as raw material through esterification reaction at the presence of catalyst, the raw material mol ratio of linalool / acetic anhydride is 1 / 1.5-1 / 3, the consumption of catalyst is 0.02-0.05 wt% of the total amount of the reactants, and the catalyst is methyl modified melamine with the formula discloses in the specification, wherein R1, R2, R2', R3 or R3' is H or methyl.

Description

technical field [0001] The invention relates to a method for preparing linalyl acetate by esterification reaction using linalool and acetic anhydride as raw materials. Background technique [0002] Linalyl acetate is a high-value spice, which is widely used in the spice and food flavor industries. Linalool reacts with a suitable acylating agent such as acetyl chloride, ketene, acetic acid or acetic anhydride to obtain linalyl acetate, because the raw material for preparing linalool comes from the carbon five cuts produced by petroleum cracking to produce ethylene, and ethyl The acylation ability of acid anhydride is strong and the price is relatively low, so the preparation of linalyl acetate by the reaction of linalool and acetic anhydride is the most economical method for the synthesis of linalyl acetate. [0003] In the prior art, the esterification reaction of linalool and acetic anhydride adopts acidic or basic catalyst, such as H 3 PO 4 Or phosphoric acid complex ca...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/145
Inventor 朱志庆吕自红郭世卓刘亚涛顾超然胡霞美
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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